EP0525901A2 - Compositions containing a fluoroether and use thereof - Google Patents
Compositions containing a fluoroether and use thereof Download PDFInfo
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- EP0525901A2 EP0525901A2 EP19920202303 EP92202303A EP0525901A2 EP 0525901 A2 EP0525901 A2 EP 0525901A2 EP 19920202303 EP19920202303 EP 19920202303 EP 92202303 A EP92202303 A EP 92202303A EP 0525901 A2 EP0525901 A2 EP 0525901A2
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- isoflurane
- azeotropic
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- approximately
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- 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
Definitions
- the invention relates to azeotropic and pseudo-azeotropic compositions comprising a fluorinated ether in combination with an alcohol or an ester and the uses of these compositions, in particular as a cleaning solvent.
- CFCs Fully halogenated chlorofluorinated solvents
- CFC-113 1,1,2-trichloro-1,2,2-trifluoroethane
- Solvents can be used in various ways, mainly cold or hot.
- the CFC-113 is often used for cleaning printed circuit boards, for cleaning or degreasing precision parts, especially in optics, mechanics or electronics.
- Various compositions based on CFC-113 are also conventionally used as a desiccant, in order to remove the water adsorbed on the surface of delicate parts.
- CFC-113 is used either pure or as a mixture with other compounds, in particular alkanes, alcohols or esters which increase the solvent power of the product.
- alkanes, alcohols or esters which increase the solvent power of the product.
- azeotropic type mixtures is then interesting, since the composition of the bath does not vary over time or during the various stages of the cleaning process.
- compositions based on CFC-113 have been developed for these various applications. Let us cite, by way of examples, patent BE-A-822,223, describing compositions CFC-113 / ethanol / nitromethane and patent US-A-3,539,462 concerning compositions based on CFC-113, 1,1-dichloroethane and methanol, ethanol, isopropanol, tert-butanol, 2,2-dimethylbutane or 2,3-dimethylbutane.
- CFC-113 as well as other chlorofluoroalkanes completely halogenated, is today suspected of causing environmental problems, on the one hand in the context of the destruction of the stratospheric ozone layer and on the other hand, in the context of the warming of the atmosphere (effect Greenhouse).
- ODP ozone-destroying potential
- the influence of a product on the greenhouse effect is expressed, still relative to CFC-11, by its global warming potential (GWP).
- GWP global warming potential
- the ODP for CFC-113 varies from 0.8 to 0.9 and its GWP from 1.3 to 1.4. Consequently, there is currently an urgent need to find new solvent compositions, having little or no harmful influence on the ozone layer.
- azeotropic compositions based on certain chlorofluorocarbons which are not completely halogenated known under the generic term hydrochlorofluorocarbons (HCFC) or hydrofluoroalkanes (HFA), such as 1,1-dichloro-1-fluoroethane (HCFC-141b) or 2,2-dichloro-1,1,1-trifluoroethane (HCFC-123), mixed in particular with methanol or ethanol, have been proposed (EP-A-325265; EP-A-389133; WO89 / 10984; W089 / 12118). These compounds have a much lower ODP and GWP than CFC-113.
- HCFC-141b has an ODP of around 0.10 and a GWP of less than 0.1.
- HCFC-123 has an ODP of the order of 0.02 and a GWP of less than 0.1.
- the boiling point of the various azeotropic or pseudo-azeotropic compositions comprising these compounds is however a little too low than to allow their use in current solvent cleaning devices without requiring adaptation of existing equipment.
- One of the objects of the present invention is to provide new azeotropic or pseudo-azeotropic compositions particularly effective when used as a solvent and more particularly as a surface cleaning solvent or as a degreasing agent.
- the invention also relates to such compositions having properties particularly suitable for cleaning printed circuit boards.
- Another object of the invention is to provide compositions having a boiling point sufficiently close to that of compositions based on CFC-113 that to allow their use in current devices for cleaning by solvent without requiring adaptation of the apparatus. existing.
- Yet another object of the invention is to provide such compositions having a particularly low ODP and GWP, compositions which can therefore be used in replacement of solvents based on completely halogenated chlorofluoroalkanes.
- the present invention relates to azeotropic or pseudo-azeotropic compositions comprising isoflurane and at least one alcohol or at least one ester.
- the boiling point of isoflurane at atmospheric pressure is approximately 49.5 ° C.
- isoflurane appears to be particularly interesting. It has indeed a very low ODP, of approximately 0.01 and a GWP equal to approximately 0.03.
- the alcohol is a lower alcohol, such as in particular, methanol, ethanol, propanol, isopropanol.
- a lower alcohol such as in particular, methanol, ethanol, propanol, isopropanol.
- the isoflurane / methanol and isoflurane / ethanol azeotropic or pseudo-azeotropic compositions are preferred.
- the isoflurane / methanol azeotropic or pseudo-azeotropic compositions are particularly preferred.
- the ester is an ester containing 2 to 6 carbon atoms, such as in particular methyl acetate, ethyl acetate, methyl formate, ethyl formate, ethyl propionate .
- Azeotropic or pseudo-azeotropic isoflurane / methyl acetate, isoflurane / methyl formate and isoflurane / ethyl formate compositions are preferred.
- azeotropic or pseudo-azeotropic composition is meant any mixture of two or more substances with an almost constant boiling point, which behaves as a substance. pure, that is to say the composition of the vapor produced by evaporation or by distillation is substantially identical to the composition of the liquid mixture.
- these azeotropes or pseudo-azeotropes with an almost constant boiling point, either minimum or maximum are therefore not separable by simple distillation and therefore their composition remains constant in solvent cleaning operations, as well as in operations for recovering used solvents by distillation.
- the thermodynamic state of a fluid is defined by four interdependent variables: pressure (P), temperature (T), composition of the liquid phase (X) and composition of the gas phase (Y).
- An azeotrope or a pseudo-azeotrope is a particular system with 2 or more components for which, at a given temperature and at a given pressure, X is substantially equal to Y.
- the compositions according to the invention are characterized by their compositions observed under pressure atmospheric. It goes without saying that this does not limit the compositions according to the invention to these particular compositions. It is indeed well known that an azeotrope with 2 or more constituents sees its composition and its boiling point vary depending on the pressure conditions adopted.
- Binary mixtures consisting of approximately 70 to 99.9% by weight of isoflurane and approximately 30 to 0.1% by weight of methanol form azeotropes or pseudo-azeotropes according to the invention.
- the aseotropes or pseudo-azeotropes formed by the binary mixtures consisting of approximately 85 to 99.7% by weight of isoflurane and approximately 15 to 0.3% by weight of methanol are preferred.
- Azeotropes or pseudo-azeotropes formed by binary mixtures consisting of approximately 92 to 98% by weight of isoflurane and approximately 8 to 2% by weight of methanol are particularly preferred.
- the binary composition consisting of approximately 95.8% by weight of isoflurane and approximately 4.2% by weight of methanol constitutes a true azeotrope, the boiling point of which is approximately 47 ° C. .
- This composition is very particularly preferred.
- Binary mixtures consisting of approximately 85 to 99.99% by weight of isoflurane and approximately 15 to 0.01% by weight of ethanol also form azeotropes or pseudo-azeotropes according to the invention.
- the azeotropes or pseudo-azeotropes formed by the binary mixtures consisting of approximately 90 to 99.9% by weight of isoflurane and approximately 10 to 0.1% by weight of ethanol are preferred.
- Azeotropes or pseudo-azeotropes formed by binary mixtures consisting of approximately 95 to 99.8% by weight of isoflurane and approximately 5 to 0.2% by weight of ethanol are particularly preferred.
- the binary composition consisting of approximately 99.3% by weight of isoflurane and approximately 0.7% by weight of ethanol constitutes a true azeotrope, the boiling point of which is approximately 49, 4 ° C. This composition is very particularly preferred.
- Binary mixtures consisting of approximately 25 to 85% by weight of isoflurane and approximately 75 to 15% by weight of methyl acetate also form azeotropes or pseudo-azeotropes according to the invention.
- the azeotropes or pseudo-azeotropes formed by the binary mixtures consisting of approximately 50 to 75% by weight of isoflurane and approximately 50 to 25% by weight of methyl acetate are preferred.
- Azeotropes or pseudo-azeotropes formed by binary mixtures consisting of approximately 56 to 72% by weight of isoflurane and approximately 44 to 28% by weight of methyl acetate are particularly preferred.
- the binary composition consisting of approximately 64.7% by weight of isoflurane and approximately 35.3% by weight of methyl acetate constitutes a true azeotrope, the boiling point of which is approximately 64 ° C. This composition is very particularly preferred.
- Binary mixtures consisting of approximately 70 to 99.9% by weight of isoflurane and approximately 30 to 0.1% by weight of methyl formate also form azeotropes or pseudoazeotropes according to the invention.
- the azeotropes or pseudo-azeotropes formed by the binary mixtures consisting of approximately 85 to 99.8% by weight of isoflurane and approximately 15 to 0.2% by weight of methyl formate are preferred.
- Azeotropes or pseudo-azeotropes formed by binary mixtures consisting of approximately 90 to 99.5% by weight of isoflurane and approximately 10 to 0.5% by weight of methyl formate are particularly preferred.
- the binary composition consisting of approximately 94.3% by weight of isoflurane and approximately 5.7% by weight of methyl formate constitutes a true azeotrope, the boiling point of which is approximately 50 , 0 ° C. This composition is very particularly preferred.
- Binary mixtures consisting of approximately 30 to 90% by weight of isoflurane and approximately 70 to 10% by weight of ethyl formate also form azeotropes or pseudo-azeotropes according to the invention.
- the azeotropes or pseudo-azeotropes formed by the binary mixtures consisting of approximately 40 to 80% by weight of isoflurane and approximately 60 to 20% by weight of ethyl formate are preferred.
- Azeotropes or pseudo-azeotropes formed by binary mixtures consisting of approximately 55 to 75% by weight of isoflurane and approximately 45 to 25% by weight of ethyl formate are particularly preferred.
- the binary composition consisting of approximately 65.9% by weight of isoflurane and approximately 34.1% by weight of ethyl formate constitutes a true azeotrope, the boiling point of which is approximately 59.7 ° C. This composition is very particularly preferred.
- compositions according to the invention Small amounts of other additives can also be added to the compositions according to the invention.
- the other optional additives are added in an amount of approximately 0.001 to 5% by weight of the azeotropic or pseudo-azeotropic mixture.
- compositions according to the invention have many uses.
- compositions according to the invention can be used in any solvent cleaning process without any separation of these compositions into their constituents by evaporation or by distillation. These compositions have very good compatibility with the different types of surfaces to be treated, whether metal, plastic or glass.
- compositions according to the invention are suitable for any cold cleaning operation, either simply by immersing the parts to be cleaned in the solvent, or by washing the parts with a cloth, sponge or any other object soaked in the solvent.
- steam degreasing consists in exposing, at room temperature, the object to be cleaned in the vapors of the solvent brought to the boil. By condensing on the object, the vapors of the distilled solvent eliminate grease and all other contaminations.
- the degreasing operation with steam conventionally consists first of all in immersing the part to be cleaned in the liquid solvent at the boiling temperature, possibly combined with treatment with ultrasound, which eliminates most of the soiling, then by immersing the part, at a temperature close to room temperature, in freshly distilled solvent and finally by exposing the part to solvent vapors which, by condensing thereon, produce a final rinse.
- this last step can be preceded by spraying the part with liquid solvent. Due to their azeotropic or pseudoazeotropic nature, the compositions according to the invention are particularly well suited to these cleaning processes.
- compositions according to the invention also appear to be particularly effective in methods for cleaning printed circuit boards, methods intended to remove from the surface of these cards the flux flux used in the soldering step of the electronic components and its residues.
- the cleaning of electronic parts, in particular the defluxing of printed circuit boards constitutes a particularly important cleaning operation from an industrial point of view and increasingly difficult to carry out because of the current evolution towards printed circuit boards. more and more complex and more and more dense in electronic components.
- the methods for soldering electronic components to cards use a coating of the latter with a flux of flux, followed by the passage of the card thus covered in molten solder. The flux cleans the conductive metal parts and promotes the adhesion of the solder.
- brazing fluxes consist of collophane, used alone or with certain activators. Brazing performed at high temperature causes at least partial degradation of the flux. This and its residues are removed from the surface of printed circuit boards in a particularly effective and selective manner with the compositions according to the invention, even when these fluxes are strongly activated.
- Azeotropic or pseudo-azeotropic compositions have in fact a high solvent power for the flux and its residues without, however, altering the material constituting the support of the card or the electronic components placed on it.
- the compositions according to the invention exhibit characteristics of viscosity and surface tension in particular, which are particularly well suited to this application.
- compositions according to the invention can also be used in any other process to replace the compositions based on CFC-113. They are particularly suitable as a desiccant, that is to say to remove the water adsorbed on the surface of solid objects requiring a perfectly clean surface, such as printed circuits, silicon plates, optical glasses, spare parts. timepieces and all other precision parts.
- 25 ml of pure isoflurane are heated to atmospheric pressure until boiling, then small amounts of methanol are gradually introduced into the bottle using a graduated syringe, via a side tube fitted with a septum.
- the azeotropic composition is determined by reading the change in the boiling temperature of the mixture as a function of its composition.
- the composition for which a minimum or maximum boiling point is observed is the azeotropic composition at atmospheric pressure.
- Table I shows the corrected boiling temperatures obtained for different compositions of isoflurane and methanol.
- the best estimate of the composition for which the boiling point is minimum is about 95.8% by weight of isoflurane.
- the boiling point is 47.2 ° C ⁇ 0.2 ° C for compositions containing approximately 92 to 98% by weight of isoflurane.
- Example 2 This example illustrates the azeotrope based on isoflurane and ethanol, highlighted using the same procedure as that used in Example 1.
- Table II shows the corrected boiling temperatures obtained for different compositions of isoflurane and ethanol.
- the best estimate of the composition for which the boiling point is maximum is about 99.3% by weight of isoflurane.
- the boiling point is 49.6 ° C ⁇ 0.2 ° C for compositions containing approximately from 96.5 to 100% by weight of isoflurane.
- This example illustrates the azeotrope based on isoflurane and methyl acetate, demonstrated using the same procedure as that used in Example 1.
- Table III shows the corrected boiling temperatures obtained for different compositions of isoflurane and methyl acetate.
- the best estimate of the composition for which the boiling point is maximum is about 64.7% by weight of isoflurane.
- the boiling point is 63.8 ° C ⁇ 0.2 ° C for compositions containing approximately from 57 to 71% by weight of isoflurane.
- This example illustrates the azeotrope based on isoflurane and methyl formate, demonstrated using the same procedure as that used in Example 1.
- Table IV shows the corrected boiling temperatures obtained for different compositions of isoflurane and methyl formate.
- the best estimate of the composition for which the boiling point is maximum is about 94.3% by weight of isoflurane.
- the boiling point is 49.9 ° C ⁇ 0.2 ° C for compositions containing approximately 90 to 98% by weight of isoflurane.
- This example illustrates the azeotrope based on isoflurane and ethyl formate, demonstrated using the same procedure. than that used in Example 1.
- Table V shows the corrected boiling temperatures obtained for different compositions of isoflurane and ethyl formate.
- the best estimate of the composition for which the boiling point is maximum is about 65.9% by weight of isoflurane.
- the boiling point is 59.5 ° C ⁇ 0.2 ° C for compositions containing approximately from 56 to 73% by weight of isoflurane.
- Printed circuit boards loaded with rosin solder flux residues of the FSW 26 type according to the DIN 8511 classification and of the RMA type according to the MIL-F-14256 specifications were treated with different defluxing compositions in a simulating laboratory apparatus. a 3-bedroom cleaning unit. Each card is first immersed for 3 minutes in 80 ml of the hot solvent mixture, under ultrasound, is then transferred to a bath of the same composition at room temperature, where it remains again for 3 minutes, then finally is maintained for 1 minute in the vapors of the cleaning composition brought to a boil.
- the effectiveness of the defluxing compositions is estimated on the one hand, by appraising the appearance of the cards by means of an optical microscope magnifying 30 X and on the other hand, by measuring the ionic residue.
- This measurement of residual ionic impurities is carried out by extraction of these residual impurities by washing the cards in an isopropanol / water bath (75/25% volume), then measurement of the electrical conductivity of the bath.
- the content of ionic residues is expressed in ⁇ gram NaCl equivalents per cm2 of printed circuit board surface (eq ⁇ g / cm2).
- Optical glasses, silicon plates, parts made of aluminum and polyethylene parts were treated in a drying installation comprising 4 successive stages (spraying / immersion / spraying / treatment with vapors) using a composition 95.6% by weight isoflurane / 4.4% by weight methanol.
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Abstract
Description
L'invention concerne des compositions azéotropiques et pseudo-azéotropiques comprenant un éther fluoré en combinaison avec un alcool ou un ester et les utilisations de ces compositions, notamment comme solvant de nettoyage.The invention relates to azeotropic and pseudo-azeotropic compositions comprising a fluorinated ether in combination with an alcohol or an ester and the uses of these compositions, in particular as a cleaning solvent.
Les solvants chlorofluorés complètement halogénés (CFC), tels que le 1,1,2-trichloro-1,2,2-trifluoroéthane (CFC-113), sont largement utilisés dans l'industrie pour le dégraissage et le nettoyage de surfaces diverses, particulièrement pour les pièces compliquées et difficiles à nettoyer. Les solvants peuvent être mis en oeuvre de différentes manières, principalement à froid ou à chaud.Fully halogenated chlorofluorinated solvents (CFCs), such as 1,1,2-trichloro-1,2,2-trifluoroethane (CFC-113), are widely used in the industry for degreasing and cleaning of various surfaces, especially for complicated and difficult to clean parts. Solvents can be used in various ways, mainly cold or hot.
Le CFC-113 est souvent utilisé pour le nettoyage des cartes de circuits imprimés, pour le nettoyage ou le dégraissage de pièces de précision, notamment en optique, en mécanique ou en électronique. Différentes compositions à base de CFC-113 sont aussi classiquement utilisées comme agent dessicatif, afin d'éliminer l'eau adsorbée à la surface de pièces délicates.The CFC-113 is often used for cleaning printed circuit boards, for cleaning or degreasing precision parts, especially in optics, mechanics or electronics. Various compositions based on CFC-113 are also conventionally used as a desiccant, in order to remove the water adsorbed on the surface of delicate parts.
Le CFC-113 est utilisé soit pur, soit en mélange avec d'autres composés, notamment des alcanes, des alcools ou des esters qui augmentent le pouvoir solvant du produit. L'emploi de mélanges de type azéotropique est alors intéressant, puisque la composition du bain ne varie pas au cours du temps ni au cours des différentes étapes du procédé de nettoyage.CFC-113 is used either pure or as a mixture with other compounds, in particular alkanes, alcohols or esters which increase the solvent power of the product. The use of azeotropic type mixtures is then interesting, since the composition of the bath does not vary over time or during the various stages of the cleaning process.
De nombreuses compositions à base de CFC-113 ont été développées en vue de ces diverses applications. Citons, à titre d'exemples, le brevet BE-A-822.223, décrivant des compositions CFC-113/éthanol/nitrométhane et le brevet US-A-3,539,462 concernant des compositions à base de CFC-113, de 1,1-dichloroéthane et de méthanol, d'éthanol, d'isopropanol, de tert-butanol, de 2,2-dimethylbutane ou de 2,3-diméthylbutane.Numerous compositions based on CFC-113 have been developed for these various applications. Let us cite, by way of examples, patent BE-A-822,223, describing compositions CFC-113 / ethanol / nitromethane and patent US-A-3,539,462 concerning compositions based on CFC-113, 1,1-dichloroethane and methanol, ethanol, isopropanol, tert-butanol, 2,2-dimethylbutane or 2,3-dimethylbutane.
Toutefois, le CFC-113, de même que d'autres chlorofluoroalcanes complètement halogénés, est aujourd'hui suspecté de provoquer des problèmes d'environnement, d'une part dans le cadre de la destruction de la couche d'ozone stratosphérique et d'autre part, dans le cadre du réchauffement de l'atmosphère (effet de serre). L'influence qu'un produit peut avoir sur la couche d'ozone, relativement au CFC-11, a été quantifiée, à partir de modèles mathématiques complexes, par son potentiel destructeur de l'ozone (ODP). L'influence d'un produit sur l'effet de serre est exprimé, toujours relativement au CFC-11, par son potentiel de réchauffement global (GWP). Selon le modèle retenu, l'ODP du CFC-113 varie de 0,8 à 0,9 et son GWP de 1,3 à 1,4. En conséquence, il y a actuellement un besoin urgent de trouver de nouvelles compositions solvantes, ayant peu ou pas d'influence néfaste sur la couche d'ozone.However, CFC-113, as well as other chlorofluoroalkanes completely halogenated, is today suspected of causing environmental problems, on the one hand in the context of the destruction of the stratospheric ozone layer and on the other hand, in the context of the warming of the atmosphere (effect Greenhouse). The influence that a product can have on the ozone layer, relative to CFC-11, has been quantified, from complex mathematical models, by its ozone-destroying potential (ODP). The influence of a product on the greenhouse effect is expressed, still relative to CFC-11, by its global warming potential (GWP). Depending on the model chosen, the ODP for CFC-113 varies from 0.8 to 0.9 and its GWP from 1.3 to 1.4. Consequently, there is currently an urgent need to find new solvent compositions, having little or no harmful influence on the ozone layer.
A cette fin, un certain nombre de compositions azéotropiques à base de certains chlorofluorocarbones non complètement halogénés, connus sous le terme générique hydrochlorofluorocarbones (HCFC) ou hydrofluoroalcanes (HFA), tels le 1,1-dichloro-1-fluoroéthane (HCFC-141b) ou le 2,2-dichloro-1,1,1-trifluoroéthane (HCFC-123), en mélange notamment avec le méthanol ou l'éthanol, ont été proposées (EP-A-325265; EP-A-389133; W089/10984; W089/12118). Ces composés présentent un ODP et un GWP beaucoup plus faibles que le CFC-113. Le HCFC-141b possède un ODP de l'ordre de 0,10 et un GWP inférieur à 0,1. Le HCFC-123 possède un ODP de l'ordre de 0,02 et un GWP inférieur à 0,1. La température d'ébullition des différentes compositions azéotropiques ou pseudo-azéotropiques comprenant ces composés est cependant un peu trop basse que pour permettre leur utilisation dans les dispositifs actuels de nettoyage par solvant sans nécessiter d'adaptation des appareillages existants.To this end, a number of azeotropic compositions based on certain chlorofluorocarbons which are not completely halogenated, known under the generic term hydrochlorofluorocarbons (HCFC) or hydrofluoroalkanes (HFA), such as 1,1-dichloro-1-fluoroethane (HCFC-141b) or 2,2-dichloro-1,1,1-trifluoroethane (HCFC-123), mixed in particular with methanol or ethanol, have been proposed (EP-A-325265; EP-A-389133; WO89 / 10984; W089 / 12118). These compounds have a much lower ODP and GWP than CFC-113. HCFC-141b has an ODP of around 0.10 and a GWP of less than 0.1. HCFC-123 has an ODP of the order of 0.02 and a GWP of less than 0.1. The boiling point of the various azeotropic or pseudo-azeotropic compositions comprising these compounds is however a little too low than to allow their use in current solvent cleaning devices without requiring adaptation of existing equipment.
Par ailleurs, il est connu, par le brevet BE-764791, que l'isoflurane (oxyde de 1-chloro-2,2,2-trifluoroéthyle et de difluorométhyle), utilisé principalement comme anesthésique, peut aussi être mis en oeuvre comme dissolvant ou comme dégraissant.Furthermore, it is known from patent BE-764791 that isoflurane (1-chloro-2,2,2-trifluoroethyl and difluoromethyl oxide), used mainly as an anesthetic, can also be used as a solvent or as a degreaser.
Un des objets de la présente invention est de fournir de nouvelles compositions azéotropiques ou pseudo-azéotropiques particulièrement performantes lorsqu'elles sont utilisées comme solvant et plus particulièrement comme solvant de nettoyage de surfaces ou comme agent dégraissant. L'invention a encore pour objet de telles compositions possédant des propriétés particulièrement adaptées au nettoyage des cartes de circuits imprimés. Un autre objet de l'invention est de fournir des compositions présentant un point d'ébullition suffisamment proche de celui des compositions à base de CFC-113 que pour permettre leur utilisation dans les dispositifs actuels de nettoyage par solvant sans nécessiter d'adaptation des appareillages existants. Encore un autre objet de l'invention est de fournir de telles compositions présentant un ODP et un GWP particulièrement faibles, compositions dès lors utilisables en remplacement des solvants à base de chlorofluoroalcanes complètement halogénés.One of the objects of the present invention is to provide new azeotropic or pseudo-azeotropic compositions particularly effective when used as a solvent and more particularly as a surface cleaning solvent or as a degreasing agent. The invention also relates to such compositions having properties particularly suitable for cleaning printed circuit boards. Another object of the invention is to provide compositions having a boiling point sufficiently close to that of compositions based on CFC-113 that to allow their use in current devices for cleaning by solvent without requiring adaptation of the apparatus. existing. Yet another object of the invention is to provide such compositions having a particularly low ODP and GWP, compositions which can therefore be used in replacement of solvents based on completely halogenated chlorofluoroalkanes.
La présente invention concerne des compositions azéotropiques ou pseudo-azéotropiques comprenant l'isoflurane et au moins un alcool ou au moins un ester. Le point d'ébullition de l'isoflurane à pression atmosphérique est environ égal à 49,5 °C. En ce qui concerne son impact sur l'environnement, l'isoflurane apparaît particulièrement intéressant. Il présente en effet un ODP très faible, d'environ 0,01 et un GWP égal à environ 0,03.The present invention relates to azeotropic or pseudo-azeotropic compositions comprising isoflurane and at least one alcohol or at least one ester. The boiling point of isoflurane at atmospheric pressure is approximately 49.5 ° C. With regard to its impact on the environment, isoflurane appears to be particularly interesting. It has indeed a very low ODP, of approximately 0.01 and a GWP equal to approximately 0.03.
De préférence, l'alcool est un alcool inférieur, tel que notamment, le méthanol, l'éthanol, le propanol, l'isopropanol. Les compositions azéotropiques ou pseudo-azéotropiques isoflurane/méthanol et isoflurane/éthanol sont préférées. Les compositions azéotropiques ou pseudo-azéotropiques isoflurane/méthanol sont particulièrement préférées.Preferably, the alcohol is a lower alcohol, such as in particular, methanol, ethanol, propanol, isopropanol. The isoflurane / methanol and isoflurane / ethanol azeotropic or pseudo-azeotropic compositions are preferred. The isoflurane / methanol azeotropic or pseudo-azeotropic compositions are particularly preferred.
De préférence, l'ester est un ester renfermant de 2 à 6 atomes de carbone, tel que notamment l'acétate de méthyle, l'acétate d'éthyle, le formiate de méthyle, le formiate d'éthyle, le propionate d'éthyle. Les compositions azéotropiques ou pseudo-azéotropiques isoflurane/acétate de méthyle, isoflurane/formiate de méthyle et isoflurane/formiate d'éthyle sont préférées.Preferably, the ester is an ester containing 2 to 6 carbon atoms, such as in particular methyl acetate, ethyl acetate, methyl formate, ethyl formate, ethyl propionate . Azeotropic or pseudo-azeotropic isoflurane / methyl acetate, isoflurane / methyl formate and isoflurane / ethyl formate compositions are preferred.
Par composition azéotropique ou pseudo-azéotropique, on entend tout mélange de deux ou plusieurs substances à point d'ébullition quasi constant, qui se comporte code une substance pure, c'est-à-dire dont la composition de la vapeur produite par évaporation ou par distillation est substantiellement identique à la composition du mélange liquide. En pratique, ces azéotropes ou pseudo-azéotropes à point d'ébullition quasi constant, soit minimum soit maximum, ne sont donc pas séparables par simple distillation et dès lors leur composition reste constante dans les opérations de nettoyage par solvant, ainsi que dans les opérations de récupération de solvants usagés par distillation. Fondamentalement, l'état thermodynamique d'un fluide est défini par quatre variables interdépendantes : la pression (P), la température (T), la composition de la phase liquide (X) et la composition de la phase gazeuse (Y). Un azéotrope ou un pseudo-azéotrope est un système particulier à 2 ou plusieurs composants pour lequel, à une température donnée et à une pression donnée, X est substantiellement égal à Y. Les compositions selon l'invention sont caractérisées par leurs compositions observées à pression atmosphérique. Il va sans dire que cela ne limite pas les compositions selon l'invention à ces compositions particulières. Il est en effet bien connu qu'un azéotrope à 2 ou plusieurs constituants voit sa composition et son point d'ébullition varier en fonction des conditions de pression retenues.By azeotropic or pseudo-azeotropic composition is meant any mixture of two or more substances with an almost constant boiling point, which behaves as a substance. pure, that is to say the composition of the vapor produced by evaporation or by distillation is substantially identical to the composition of the liquid mixture. In practice, these azeotropes or pseudo-azeotropes with an almost constant boiling point, either minimum or maximum, are therefore not separable by simple distillation and therefore their composition remains constant in solvent cleaning operations, as well as in operations for recovering used solvents by distillation. Basically, the thermodynamic state of a fluid is defined by four interdependent variables: pressure (P), temperature (T), composition of the liquid phase (X) and composition of the gas phase (Y). An azeotrope or a pseudo-azeotrope is a particular system with 2 or more components for which, at a given temperature and at a given pressure, X is substantially equal to Y. The compositions according to the invention are characterized by their compositions observed under pressure atmospheric. It goes without saying that this does not limit the compositions according to the invention to these particular compositions. It is indeed well known that an azeotrope with 2 or more constituents sees its composition and its boiling point vary depending on the pressure conditions adopted.
Les mélanges binaires constitués d'environ 70 à 99,9 % en poids d'isoflurane et d'environ 30 à 0,1 % en poids de méthanol forment des azéotropes ou des pseudo-azéotropes selon l'invention. Les aséotropes ou les pseudo-azéotropes formés par les mélanges binaires constitués d'environ 85 à 99,7 % en poids d'isoflurane et d'environ 15 à 0,3 % en poids de méthanol sont préférés. Les azéotropes ou les pseudo-azéotropes formés par les mélanges binaires constitués d'environ 92 à 98 % en poids d'isoflurane et d'environ 8 à 2 % en poids de méthanol sont particulièrement préférés. A pression atmosphérique, la composition binaire constituée d'environ 95,8 % en poids d'isoflurane et d'environ 4,2 % en poids de méthanol constitue un azéotrope vrai, dont le point d'ébullition est d'environ 47 °C. Cette composition est tout particulièrement préférée.Binary mixtures consisting of approximately 70 to 99.9% by weight of isoflurane and approximately 30 to 0.1% by weight of methanol form azeotropes or pseudo-azeotropes according to the invention. The aseotropes or pseudo-azeotropes formed by the binary mixtures consisting of approximately 85 to 99.7% by weight of isoflurane and approximately 15 to 0.3% by weight of methanol are preferred. Azeotropes or pseudo-azeotropes formed by binary mixtures consisting of approximately 92 to 98% by weight of isoflurane and approximately 8 to 2% by weight of methanol are particularly preferred. At atmospheric pressure, the binary composition consisting of approximately 95.8% by weight of isoflurane and approximately 4.2% by weight of methanol constitutes a true azeotrope, the boiling point of which is approximately 47 ° C. . This composition is very particularly preferred.
Les mélanges binaires constitués d'environ 85 à 99,99 % en poids d'isoflurane et d'environ 15 à 0,01 % en poids d'éthanol forment aussi des azéotropes ou des pseudo-azéotropes selon l'invention. Les azéotropes ou les pseudo-azéotropes formés par les mélanges binaires constitués d'environ 90 à 99,9 % en poids d'isoflurane et d'environ 10 à 0,1 % en poids d'éthanol sont préférés. Les azéotropes ou les pseudo-azéotropes formés par les mélanges binaires constitués d'environ 95 à 99,8 % en poids d'isoflurane et d'environ 5 à 0,2 % en poids d'éthanol sont particulièrement préférés. A pression atmosphérique, la composition binaire constituée d'environ 99,3 % en poids d'isoflurane et d'environ 0,7 % en poids d'éthanol constitue un azéotrope vrai, dont le point d'ébullition est d'environ 49,4 °C. Cette composition est tout particulièrement préférée.Binary mixtures consisting of approximately 85 to 99.99% by weight of isoflurane and approximately 15 to 0.01% by weight of ethanol also form azeotropes or pseudo-azeotropes according to the invention. The azeotropes or pseudo-azeotropes formed by the binary mixtures consisting of approximately 90 to 99.9% by weight of isoflurane and approximately 10 to 0.1% by weight of ethanol are preferred. Azeotropes or pseudo-azeotropes formed by binary mixtures consisting of approximately 95 to 99.8% by weight of isoflurane and approximately 5 to 0.2% by weight of ethanol are particularly preferred. At atmospheric pressure, the binary composition consisting of approximately 99.3% by weight of isoflurane and approximately 0.7% by weight of ethanol constitutes a true azeotrope, the boiling point of which is approximately 49, 4 ° C. This composition is very particularly preferred.
Les mélanges binaires constitués d'environ 25 à 85 % en poids d'isoflurane et d'environ 75 à 15 % en poids d'acétate de méthyle forment aussi des azéotropes ou des pseudo-azéotropes selon l'invention. Les azéotropes ou les pseudo-azéotropes formés par les mélanges binaires constitués d'environ 50 à 75 % en poids d'isoflurane et d'environ 50 à 25 % en poids d'acétate de méthyle sont préférés. Les azéotropes ou les pseudo-azéotropes formés par les mélanges binaires constitués d'environ 56 à 72 % en poids d'isoflurane et d'environ 44 à 28 % en poids d'acétate de méthyle sont particulièrement préférés. A pression atmosphérique, la composition binaire constituée d'environ 64,7 % en poids d'isoflurane et d'environ 35,3 % en poids d'acétate de méthyle constitue un azéotrope vrai, dont le point d'ébullition est d'environ 64 °C. Cette composition est tout particulièrement préférée.Binary mixtures consisting of approximately 25 to 85% by weight of isoflurane and approximately 75 to 15% by weight of methyl acetate also form azeotropes or pseudo-azeotropes according to the invention. The azeotropes or pseudo-azeotropes formed by the binary mixtures consisting of approximately 50 to 75% by weight of isoflurane and approximately 50 to 25% by weight of methyl acetate are preferred. Azeotropes or pseudo-azeotropes formed by binary mixtures consisting of approximately 56 to 72% by weight of isoflurane and approximately 44 to 28% by weight of methyl acetate are particularly preferred. At atmospheric pressure, the binary composition consisting of approximately 64.7% by weight of isoflurane and approximately 35.3% by weight of methyl acetate constitutes a true azeotrope, the boiling point of which is approximately 64 ° C. This composition is very particularly preferred.
Les mélanges binaires constitués d'environ 70 à 99,9 % en poids d'isoflurane et d'environ 30 à 0,1 % en poids de formiate de méthyle forment aussi des azéotropes ou des pseudoazéotropes selon l'invention. Les azéotropes ou les pseudo-azéotropes formés par les mélanges binaires constitués d'environ 85 à 99,8 % en poids d'isoflurane et d'environ 15 à 0,2 % en poids de formiate de méthyle sont préférés. Les azéotropes ou les pseudo-azéotropes formés par les mélanges binaires constitués d'environ 90 à 99,5 % en poids d'isoflurane et d'environ 10 à 0,5 % en poids de formiate de méthyle sont particulièrement préférés. A pression atmosphérique, la composition binaire constituée d'environ 94,3 % en poids d'isoflurane et d'environ 5,7 % en poids de formiate de méthyle constitue un azéotrope vrai, dont le point d'ébullition est d'environ 50,0 °C. Cette composition est tout particulièrement préférée.Binary mixtures consisting of approximately 70 to 99.9% by weight of isoflurane and approximately 30 to 0.1% by weight of methyl formate also form azeotropes or pseudoazeotropes according to the invention. The azeotropes or pseudo-azeotropes formed by the binary mixtures consisting of approximately 85 to 99.8% by weight of isoflurane and approximately 15 to 0.2% by weight of methyl formate are preferred. Azeotropes or pseudo-azeotropes formed by binary mixtures consisting of approximately 90 to 99.5% by weight of isoflurane and approximately 10 to 0.5% by weight of methyl formate are particularly preferred. At atmospheric pressure, the binary composition consisting of approximately 94.3% by weight of isoflurane and approximately 5.7% by weight of methyl formate constitutes a true azeotrope, the boiling point of which is approximately 50 , 0 ° C. This composition is very particularly preferred.
Les mélanges binaires constitués d'environ 30 à 90 % en poids d'isoflurane et d'environ 70 à 10 % en poids de formiate d'éthyle forment aussi des azéotropes ou des pseudo-azéotropes selon l'invention. Les azéotropes ou les pseudo-azéotropes formés par les mélanges binaires constitués d'environ 40 à 80 % en poids d'isoflurane et d'environ 60 à 20 % en poids de formiate d'éthyle sont préférés. Les azéotropes ou les pseudo-azéotropes formés par les mélanges binaires constitués d'environ 55 à 75 % en poids d'isoflurane et d'environ 45 à 25 % en poids de formiate d'éthyle sont particulièrement préférés. A pression atmosphérique, la composition binaire constituée d'environ 65,9 % en poids d'isoflurane et d'environ 34,1 % en poids de formiate d'éthyle constitue un azéotrope vrai, dont le point d'ébullition est d'environ 59,7 °C. Cette composition est tout particulièrement préférée.Binary mixtures consisting of approximately 30 to 90% by weight of isoflurane and approximately 70 to 10% by weight of ethyl formate also form azeotropes or pseudo-azeotropes according to the invention. The azeotropes or pseudo-azeotropes formed by the binary mixtures consisting of approximately 40 to 80% by weight of isoflurane and approximately 60 to 20% by weight of ethyl formate are preferred. Azeotropes or pseudo-azeotropes formed by binary mixtures consisting of approximately 55 to 75% by weight of isoflurane and approximately 45 to 25% by weight of ethyl formate are particularly preferred. At atmospheric pressure, the binary composition consisting of approximately 65.9% by weight of isoflurane and approximately 34.1% by weight of ethyl formate constitutes a true azeotrope, the boiling point of which is approximately 59.7 ° C. This composition is very particularly preferred.
De petites quantités d'autres additifs peuvent également être ajoutées aux compositions selon l'invention. On peut ainsi leur ajouter des stabilisants, des agents tensioactifs ou tous autres additifs permettant d'améliorer leurs performances lors de leur utilisation. Les autres additifs éventuels sont ajoutés à raison d'environ 0,001 à 5 % en poids du mélange azéotropique ou pseudo-azéotropique.Small amounts of other additives can also be added to the compositions according to the invention. One can thus add stabilizers, surfactants or any other additives to improve their performance during their use. The other optional additives are added in an amount of approximately 0.001 to 5% by weight of the azeotropic or pseudo-azeotropic mixture.
Les compositions selon l'invention ont de nombreux usages.The compositions according to the invention have many uses.
De par leur nature azéotropique ou pseudo-azéotropique, les compositions selon l'invention peuvent être utilisées dans tout procédé de nettoyage par solvant sans qu'une séparation de ces compositions en leurs constituants n'intervienne par évaporation ou par distillation. Ces compositions présentent une très bonne compatibilité avec les différents types de surfaces à traiter, qu'elles soient en métal, en plastique ou en verre.Due to their azeotropic or pseudo-azeotropic nature, the compositions according to the invention can be used in any solvent cleaning process without any separation of these compositions into their constituents by evaporation or by distillation. These compositions have very good compatibility with the different types of surfaces to be treated, whether metal, plastic or glass.
Les compositions selon l'invention conviennent pour toute opération de nettoyage à froid, soit simplement par immersion des pièces à nettoyer dans le solvant, soit par lavage des pièces avec un chiffon, une éponge ou tout autre objet trempé dans le solvant.The compositions according to the invention are suitable for any cold cleaning operation, either simply by immersing the parts to be cleaned in the solvent, or by washing the parts with a cloth, sponge or any other object soaked in the solvent.
Un autre domaine d'applications pour lequel les compositions selon l'invention sont particulièrement intéressantes est le nettoyage de surfaces à la vapeur. Dans sa forme la plus simple, le dégraissage à la vapeur consiste en l'exposition, à température ambiante, de l'objet à nettoyer dans les vapeurs du solvant porté à ébullition. En se condensant sur l'objet, les vapeurs du solvant distillé éliminent les graisses et toutes autres contaminations.Another field of applications for which the compositions according to the invention are particularly advantageous is the cleaning of surfaces with steam. In its simplest form, steam degreasing consists in exposing, at room temperature, the object to be cleaned in the vapors of the solvent brought to the boil. By condensing on the object, the vapors of the distilled solvent eliminate grease and all other contaminations.
Pour les salissures plus difficiles à éliminer, nécessitant un traitement à température plus élevée afin d'améliorer le pouvoir nettoyant du solvant, ou pour les grandes installations de nettoyage dans lesquelles le nettoyage des pièces métalliques ou des assemblages doit être réalisé efficacement et rapidement, l'opération de dégraissage à la vapeur consiste, classiquement, d'abord en l'immersion de la pièce à nettoyer dans le solvant liquide à la température d'ébullition, éventuellement conjuguée à un traitement par des ultrasons, ce qui élimine la majeure partie des salissures, ensuite en l'immersion de la pièce, à une température proche de la température ambiante, dans du solvant fraîchement distillé et finalement en l'exposition de la pièce à des vapeurs du solvant qui, en se condensant sur celle-ci, réalisent un rinçage final. Eventuellement, cette dernière étape peut être précédée d'une aspersion de la pièce par du solvant liquide. En raison de leur caractère azéotropique ou pseudoazéotropique, les compositions selon l'invention sont particulièrement bien adaptées à ces procédés de nettoyage.For dirt that is more difficult to remove, requiring treatment at a higher temperature in order to improve the cleaning power of the solvent, or for large cleaning installations in which the cleaning of metal parts or assemblies must be carried out efficiently and quickly, l the degreasing operation with steam conventionally consists first of all in immersing the part to be cleaned in the liquid solvent at the boiling temperature, possibly combined with treatment with ultrasound, which eliminates most of the soiling, then by immersing the part, at a temperature close to room temperature, in freshly distilled solvent and finally by exposing the part to solvent vapors which, by condensing thereon, produce a final rinse. Optionally, this last step can be preceded by spraying the part with liquid solvent. Due to their azeotropic or pseudoazeotropic nature, the compositions according to the invention are particularly well suited to these cleaning processes.
Les compositions selon l'invention apparaissent également particulièrement efficaces dans des procédés de nettoyage de cartes de circuits imprimés, procédés destinés à éliminer de la surface de ces cartes le flux décapant utilisé dans l'étape de soudure des composants électroniques et ses résidus. Le nettoyage de pièces électroniques, notamment le défluxage des cartes de circuits imprimés constitue une opération de nettoyage particulièrement importante d'un point de vue industriel et de plus en plus délicate à réaliser en raison de l'évolution actuelle vers des cartes de circuits imprimés de plus en plus complexes et de plus en plus denses en composants électroniques. Classiquement, les procédés de soudure des composants électroniques sur les cartes mettent en oeuvre un coating de celles-ci avec un flux décapant, suivi du passage de la carte ainsi recouverte dans une brasure fondue. Le flux nettoie les parties métalliques conductrices et favorise l'adhérence de la brasure. Des flux de brasage classiques sont constitués de collophane, utilisée seule ou avec certains activants. Le brasage réalisé à température élevée provoque une dégradation au moins partielle du flux. Celui-ci et ses résidus sont éliminés de la surface des cartes de circuits imprimés de manière particulièrement efficace et sélective avec les compositions selon l'invention, même lorsque ces flux sont fortement activés. Les compositions azéotropiques ou pseudo-azéotropiques possèdent en effet un pouvoir solvant élevé pour le flux et ses résidus sans cependant altérer le matériau constituant le support de la carte ni les composants électroniques disposés sur celle-ci. En outre, les compositions selon l'invention présentent des caractéristiques de viscosité et de tension superficielle notamment, particulièrement bien adaptées à cette application.The compositions according to the invention also appear to be particularly effective in methods for cleaning printed circuit boards, methods intended to remove from the surface of these cards the flux flux used in the soldering step of the electronic components and its residues. The cleaning of electronic parts, in particular the defluxing of printed circuit boards constitutes a particularly important cleaning operation from an industrial point of view and increasingly difficult to carry out because of the current evolution towards printed circuit boards. more and more complex and more and more dense in electronic components. Conventionally, the methods for soldering electronic components to cards use a coating of the latter with a flux of flux, followed by the passage of the card thus covered in molten solder. The flux cleans the conductive metal parts and promotes the adhesion of the solder. Conventional brazing fluxes consist of collophane, used alone or with certain activators. Brazing performed at high temperature causes at least partial degradation of the flux. This and its residues are removed from the surface of printed circuit boards in a particularly effective and selective manner with the compositions according to the invention, even when these fluxes are strongly activated. Azeotropic or pseudo-azeotropic compositions have in fact a high solvent power for the flux and its residues without, however, altering the material constituting the support of the card or the electronic components placed on it. In addition, the compositions according to the invention exhibit characteristics of viscosity and surface tension in particular, which are particularly well suited to this application.
Les compositions selon l'invention peuvent également être utilisées dans tout autre procédé en remplacement des compositions à base de CFC-113. Elles conviennent particulièrement bien comme agent dessicatif, c'est-à-dire pour éliminer l'eau adsorbée à la surface d'objets solides nécessitant une surface parfaitement propre, tels que circuits imprimés, plaques au silicium, verres d'optique, pièces détachées d'horlogerie et toutes autres pièces de précision.The compositions according to the invention can also be used in any other process to replace the compositions based on CFC-113. They are particularly suitable as a desiccant, that is to say to remove the water adsorbed on the surface of solid objects requiring a perfectly clean surface, such as printed circuits, silicon plates, optical glasses, spare parts. timepieces and all other precision parts.
Les exemples ci-après, non limitatifs, illustrent l'invention de manière plus détaillée.The following non-limiting examples illustrate the invention in more detail.
Pour mettre en évidence l'existence de compositions azéotropiques ou pseudo-azéotropiques entre l'isoflurane et le méthanol, on a utilisé un appareillage en verre constitué d'un flacon bouilleur surmonté d'un condenseur à reflux. La température du liquide est mesurée au moyen d'un thermomètre plongeant dans le flacon.To demonstrate the existence of azeotropic or pseudo-azeotropic compositions between isoflurane and methanol, glass apparatus consisting of a boiling flask surmounted by a reflux condenser was used. The temperature of the liquid is measured using a thermometer immersed in the bottle.
25 ml d'isoflurane pur sont chauffés à la pression atmosphérique jusqu'à ébullition, puis de petites quantités de méthanol sont progressivement introduites dans le flacon au moyen d'une seringue graduée, via une tubulure latérale équipée d'un septum.25 ml of pure isoflurane are heated to atmospheric pressure until boiling, then small amounts of methanol are gradually introduced into the bottle using a graduated syringe, via a side tube fitted with a septum.
La détermination de la composition azéotropique se fait par relevé de l'évolution de la température d'ébullition du mélange en fonction de sa composition. La composition pour laquelle est observé un point d'ébullition minimum ou maximum est la composition azéotropique à la pression atmosphérique.The azeotropic composition is determined by reading the change in the boiling temperature of the mixture as a function of its composition. The composition for which a minimum or maximum boiling point is observed is the azeotropic composition at atmospheric pressure.
L'influence de la pression atmosphérique sur la température d'ébullition des mélanges est corrigée à l'aide de la formule suivante :
avec tr, la température relevée en °C
tc, la température corrigée en °C
P, la pression atmosphérique au moment de la mesure, en mm Hg.The influence of atmospheric pressure on the boiling point of mixtures is corrected using the following formula:
with tr, the temperature recorded in ° C
tc, the corrected temperature in ° C
P, the atmospheric pressure at the time of the measurement, in mm Hg.
Le tableau I rassemble les températures d'ébullition corrigées, obtenues pour différentes compositions d'isoflurane et de méthanol. Table I shows the corrected boiling temperatures obtained for different compositions of isoflurane and methanol.
La meilleure estimation de la composition pour laquelle le point d'ébullition est minimum est d'environ 95,8 % en poids d'isoflurane. Le point d'ébullition est de 47,2 °C ± 0,2 °C pour des compositions contenant environ de 92 à 98 % en poids d'isoflurane.The best estimate of the composition for which the boiling point is minimum is about 95.8% by weight of isoflurane. The boiling point is 47.2 ° C ± 0.2 ° C for compositions containing approximately 92 to 98% by weight of isoflurane.
Cet exemple illustre l'azéotrope à base d'isoflurane et d'éthanol, mis en évidence à l'aide de la même procédure que celle utilisée dans l'exemple 1.This example illustrates the azeotrope based on isoflurane and ethanol, highlighted using the same procedure as that used in Example 1.
Le tableau II rassemble les températures d'ébullition corrigées, obtenues pour différentes compositions d'isoflurane et d'éthanol. Table II shows the corrected boiling temperatures obtained for different compositions of isoflurane and ethanol.
La meilleure estimation de la composition pour laquelle le point d'ébullition est maximum est d'environ 99,3 % en poids d'isoflurane. Le point d'ébullition est de 49,6 °C ± 0,2 °C pour des compositions contenant environ de 96,5 à 100 % en poids d'isoflurane.The best estimate of the composition for which the boiling point is maximum is about 99.3% by weight of isoflurane. The boiling point is 49.6 ° C ± 0.2 ° C for compositions containing approximately from 96.5 to 100% by weight of isoflurane.
Cet exemple illustre l'azéotrope à base d'isoflurane et d'acétate de méthyle, mis en évidence à l'aide de la même procédure que celle utilisée dans l'exemple 1.This example illustrates the azeotrope based on isoflurane and methyl acetate, demonstrated using the same procedure as that used in Example 1.
Le tableau III rassemble les températures d'ébullition corrigées, obtenues pour différentes compositions d'isoflurane et d'acétate de méthyle. Table III shows the corrected boiling temperatures obtained for different compositions of isoflurane and methyl acetate.
La meilleure estimation de la composition pour laquelle le point d'ébullition est maximum est d'environ 64,7 % en poids d'isoflurane. Le point d'ébullition est de 63,8 °C ± 0,2 °C pour des compositions contenant environ de 57 à 71 % en poids d'isoflurane.The best estimate of the composition for which the boiling point is maximum is about 64.7% by weight of isoflurane. The boiling point is 63.8 ° C ± 0.2 ° C for compositions containing approximately from 57 to 71% by weight of isoflurane.
Cet exemple illustre l'azéotrope à base d'isoflurane et de formiate de méthyle, mis en évidence à l'aide de la même procédure que celle utilisée dans l'exemple 1.This example illustrates the azeotrope based on isoflurane and methyl formate, demonstrated using the same procedure as that used in Example 1.
Le tableau IV rassemble les températures d'ébullition corrigées, obtenues pour différentes compositions d'isoflurane et de formiate de méthyle. Table IV shows the corrected boiling temperatures obtained for different compositions of isoflurane and methyl formate.
La meilleure estimation de la composition pour laquelle le point d'ébullition est maximum est d'environ 94,3 % en poids d'isoflurane. Le point d'ébullition est de 49,9 °C ± 0,2 °C pour des compositions contenant environ de 90 à 98 % en poids d'isoflurane.The best estimate of the composition for which the boiling point is maximum is about 94.3% by weight of isoflurane. The boiling point is 49.9 ° C ± 0.2 ° C for compositions containing approximately 90 to 98% by weight of isoflurane.
Cet exemple illustre l'azéotrope à base d'isoflurane et de formiate d'éthyle, mis en évidence à l'aide de la même procédure que celle utilisée dans l'exemple 1.This example illustrates the azeotrope based on isoflurane and ethyl formate, demonstrated using the same procedure. than that used in Example 1.
Le tableau V rassemble les températures d'ébullition corrigées, obtenues pour différentes compositions d'isoflurane et de formiate d'éthyle. Table V shows the corrected boiling temperatures obtained for different compositions of isoflurane and ethyl formate.
La meilleure estimation de la composition pour laquelle le point d'ébullition est maximum est d'environ 65,9 % en poids d'isoflurane. Le point d'ébullition est de 59,5 °C ± 0,2 °C pour des compositions contenant environ de 56 à 73 % en poids d'isoflurane.The best estimate of the composition for which the boiling point is maximum is about 65.9% by weight of isoflurane. The boiling point is 59.5 ° C ± 0.2 ° C for compositions containing approximately from 56 to 73% by weight of isoflurane.
Des cartes de circuits imprimés chargées de résidus de flux de soudure à la collophane de type FSW 26 suivant la classification DIN 8511 et de type RMA suivant les spécifications MIL-F-14256 ont été traitées par différentes compositions de défluxage dans un appareillage de laboratoire simulant une unité de nettoyage à 3 chambres. Chaque carte est d'abord immergée pendant 3 minutes dans 80 ml du mélange solvant chaud, sous ultrasons, est ensuite transférée dans un bain de la même composition à température ambiante, où elle séjourne de nouveau pendant 3 minutes, puis enfin est maintenue pendant 1 minute dans les vapeurs de la composition de nettoyage portée à ébullition.Printed circuit boards loaded with rosin solder flux residues of the FSW 26 type according to the DIN 8511 classification and of the RMA type according to the MIL-F-14256 specifications were treated with different defluxing compositions in a simulating laboratory apparatus. a 3-bedroom cleaning unit. Each card is first immersed for 3 minutes in 80 ml of the hot solvent mixture, under ultrasound, is then transferred to a bath of the same composition at room temperature, where it remains again for 3 minutes, then finally is maintained for 1 minute in the vapors of the cleaning composition brought to a boil.
L'efficacité des compositions de défluxage est estimée d'une part, par appréciation de l'aspect des cartes au moyen d'un microscope optique grossissant 30 X et d'autre part, par mesure du résidu ionique. Cette mesure des impuretés ioniques résiduelles est réalisée par extraction de ces impuretés résiduelles par lavage des cartes dans un bain isopropanol/eau (75/25 % volume), puis mesure de la conductibilité électrique du bain. La teneur en résidus ioniques est exprimée en équivalents µgramme NaCl par cm² de surface de carte de circuit imprimé (eq µg/cm²).The effectiveness of the defluxing compositions is estimated on the one hand, by appraising the appearance of the cards by means of an optical microscope magnifying 30 X and on the other hand, by measuring the ionic residue. This measurement of residual ionic impurities is carried out by extraction of these residual impurities by washing the cards in an isopropanol / water bath (75/25% volume), then measurement of the electrical conductivity of the bath. The content of ionic residues is expressed in µgram NaCl equivalents per cm² of printed circuit board surface (eq µg / cm²).
Les résultats obtenus avec une composition pseudo-azéotropique selon l'invention et, à titre de comparaison, avec d'autres compositions azéotropiques, sont rassemblés au tableau VI.The results obtained with a pseudo-azeotropic composition according to the invention and, for comparison, with other azeotropic compositions, are collated in Table VI .
Des verres optiques, des plaques au silicium, des pièces en aluminium et des pièces en polyéthylène ont été traitées dans une installation de séchage comportant 4 étapes successives (aspersion/immersion/aspersion/traitement par les vapeurs) au moyen d'une composition 95,6 % poids isoflurane/4,4 % poids méthanol.Optical glasses, silicon plates, parts made of aluminum and polyethylene parts were treated in a drying installation comprising 4 successive stages (spraying / immersion / spraying / treatment with vapors) using a composition 95.6% by weight isoflurane / 4.4% by weight methanol.
Les différentes surfaces obtenues après traitement sont parfaitement sèches, complètement débarrassées de toutes traces d'eau adsorbée. Après évaporation, aucun résidu de la composition de séchage ne subsiste sur les surfaces.
Claims (11)
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
BE9100711 | 1991-08-01 | ||
BE9100711A BE1005163A3 (en) | 1991-08-01 | 1991-08-01 | Composition containing fluorinated ether and use thereof. |
Publications (2)
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EP0525901A2 true EP0525901A2 (en) | 1993-02-03 |
EP0525901A3 EP0525901A3 (en) | 1993-08-11 |
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ID=3885637
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EP19920202303 Withdrawn EP0525901A3 (en) | 1991-08-01 | 1992-07-27 | Compositions containing a fluoroether and use thereof |
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US (1) | US5336429A (en) |
EP (1) | EP0525901A3 (en) |
JP (1) | JPH05202390A (en) |
BE (1) | BE1005163A3 (en) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP0583719A1 (en) * | 1992-08-17 | 1994-02-23 | Solvay Fluor und Derivate GmbH | Compositions comprising the 1-chloro-2,2,2-trifluoroethyl difluoromethyl ehter and partially fluorinated alcanols |
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US8021490B2 (en) * | 2007-01-04 | 2011-09-20 | Eastman Chemical Company | Substrate cleaning processes through the use of solvents and systems |
PL2244783T3 (en) | 2008-01-22 | 2020-08-24 | Board Of Regents, The University Of Texas System | Volatile anesthetic compositions and methods of use |
CN102014961B (en) | 2008-01-22 | 2017-10-13 | 得克萨斯大学体系董事会 | The volatile anesthetic composition containing extractant for local anaesthesia and/or pain relief |
US7736537B1 (en) * | 2008-01-24 | 2010-06-15 | Mainstream Engineering Corp. | Replacement solvents having improved properties for refrigeration flushes |
TW201012796A (en) * | 2008-09-02 | 2010-04-01 | Solvay Fluor Gmbh | Method for removal of contaminants |
EP3195896A1 (en) | 2009-05-05 | 2017-07-26 | Board of Regents, The University of Texas System | Novel formulations of volatile anesthetics and methods of use for reducing inflammation |
AU2012272933B2 (en) | 2011-06-24 | 2016-08-11 | Vapogenix, Inc. | Novel formulations and methods for treating dermatological disorders or diseases |
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- 1991-08-01 BE BE9100711A patent/BE1005163A3/en not_active IP Right Cessation
-
1992
- 1992-07-27 EP EP19920202303 patent/EP0525901A3/en not_active Withdrawn
- 1992-08-03 US US07/923,689 patent/US5336429A/en not_active Expired - Fee Related
- 1992-08-03 JP JP4206714A patent/JPH05202390A/en active Pending
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EP0583719A1 (en) * | 1992-08-17 | 1994-02-23 | Solvay Fluor und Derivate GmbH | Compositions comprising the 1-chloro-2,2,2-trifluoroethyl difluoromethyl ehter and partially fluorinated alcanols |
Also Published As
Publication number | Publication date |
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US5336429A (en) | 1994-08-09 |
EP0525901A3 (en) | 1993-08-11 |
JPH05202390A (en) | 1993-08-10 |
BE1005163A3 (en) | 1993-05-11 |
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