JP2001509533A - Azeotropic and azeotrope-like compositions of 1-bromopropane and highly fluorinated hydrocarbons - Google Patents

Abstract

(57) [Summary] The present invention provides a solvent composition containing 1-bromopropane and decafluoropentane for use as a solvent for cleaning and degreasing. Preferably, the decafluoropentane consists essentially of 1,1,1,1,2,3,4,4,5,5,5-decafluoropentane. The solvent compositions of the present invention may optionally include stabilizers and co-solvents such as alcohols, ketones, ethers, acetals, nitroalkanes, epoxides, and amines. Certain compositions comprising 1-bromopropane, 1,1,1,2,3,4,4,5,5,5-decafluoropentane and an optional stabilizer are known as cleaning and degreasing solvents. Is particularly suitable as an azeotrope composition.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001] The present application for the relevant application claims of Richard J. DeGroot 1997 July 9, with applications due to, priority to US Provisional Application No. 60 / 052,058 of co-pending. FIELD OF THE INVENTION The present invention relates to cleaning solvents comprising highly fluorinated hydrocarbons and 1-bromopropane, and to a method for cleaning articles. More specifically, the present invention relates to 1,1,1
, 2,3,4,4,5,5,5-decafluoropentene, 1-bromopropane, and optionally a solvent composition comprising a stabilizer and a cosolvent, and the surface of cloth, plastic, metal and ceramic. The present invention relates to a method for cleaning articles having the same. BACKGROUND OF THE INVENTION Chlorofluorocarbon (CHC) and hydrochlorofluorocarbon (HCF)
There is a need to find a new solvent to replace C). These solvents are commonly used as flame retardants in various applications, including cleaning and degreasing solvents for the metal, textile, and electronics industries, and as heat transfer media for refrigeration processes. Have been. Recently, the use of these solvents has been limited because of their environmental harm (especially in view of the link between their use and the destruction of the atmospheric ozone layer). Highly fluorinated hydrofluorocarbons (HFCs) are considered to be promising alternatives to CFCs and HCFCs in many applications.
HFCs are chemically stable, non-toxic, non-flammable, and less harmful to the environment than CFCs and HCFCs. However, HFCs use CFCs and HCHCs.
It does not appear to be as effective a cleaning and degreasing solvent. Highly fluorinated hydrofluorocarbons (HFCs) have a lower solvating capacity compared to CFCs and HCFCs, and may also dissolve greases and oils, or may contain other undesirable substances such as fluxes and fluxes on printed circuit boards. Residue) is not as effective as CFC or HCFC. HFCs can be combined with other organic solvents to obtain cleaning solutions with higher solvating capabilities. The organic solvent added must be carefully selected so that the resulting cleaning and degreasing solvent retains its desired physical and chemical properties (eg, low toxicity, low boiling point, environmental friendliness, and nonflammability). Must. In addition, certain solvent mixtures may initially have essentially desirable physical and chemical properties (ie, non-toxic, low boiling,
Non-flammability, and high solvation capacity), but in practice this mixture is inadequate.

[0002] Most solvent mixtures separate during use, especially when the solvent is heated during the cleaning process or during solvent recovery. When the mixture undergoes partitioning, one or more deficient solvents for its components are obtained. The properties of the solvent thus obtained are not the same as the original solvent. For example, in a steam deflux system or a steam degrease system, the solvent is often heated and boiled to vaporize the solvent composition. The vaporized solvent is removed from the components inserted into the system (
For example, on a circuit board). When separation occurs, the composition of the vaporized solvent will differ from the composition of the liquid solvent in the solvent reservoir. The result of such a separation is a solution that can adversely affect the safety and effectiveness of the cleaning operation. In order to ensure a safe and effective cleaning and degreasing process, it is advantageous to use a non-separable solvent.

In addition, it is advantageous to minimize separation during solvent recovery in order to improve efficiency and reduce costs. To obtain a substantially pure solvent that can be reused, the solvent is often recovered by distilling the spent or contaminated solution. If separation occurs during recovery, it is necessary to add one or more of the first components to the recovered solvent in order to maintain the initial solvent composition. SUMMARY OF THE INVENTION The present invention provides a solvent composition comprising highly fluorinated hydrochlorofluorocarbon (HFC) and 1-bromopropane, which is useful as a cleaning solvent and a degreasing solvent. The solvent composition of the present invention optionally includes a stabilizer and a co-solvent. Stabilizers and co-solvents include alcohols, ketones, ethers, acetals, nitroalkanes, epoxides, amines, and saturated and unsaturated hydrocarbons. When certain highly fluorinated hydrocarbons and 1-bromopropane are mixed in certain ratios, an azeotrope is formed. While azeotropes are the preferred compositions, non-azeotropes are also considered to be within the scope of the present invention. The most preferred composition for the present invention is an azeotropic composition comprising 1,1,1,1,2,3,4,4,5,5,5-decafluoropentane and 1-bromopropane. The solvent composition optionally includes a stabilizer and a co-solvent. Solvent compositions containing HFC and 1-bromopropane result in non-azeotropic and azeotropic or azeotrope-like compositions that are highly suitable for solvent cleaning applications.

[0004] The invention further provides a method for cleaning articles having a cloth, ceramic, plastic, or metal surface using a solvent composition comprising 1-bromopropane and a highly fluorinated hydrocarbon. provide. The solvent of the present invention is applied to the surface of the article by any known or conventional method to degrease grease, oil, and particulate matter adhering to the surface of the article and clean the surface. By removing the contaminated solvent, a cleaned article is obtained, which is suitable for further processing or for shipping to consumers. DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a solvent composition containing 1-bromopropane and a highly fluorinated hydrocarbon for use in cleaning and degreasing. Preferably, the highly fluorinated hydrocarbon is highly fluorinated pentane. The solvent compositions of the present invention optionally include stabilizers and co-solvents (eg, alcohols, ketones, ethers, acetals, nitroalkanes, epoxides, amines, and saturated and unsaturated hydrocarbons). The solvent composition of the present invention further includes an azeotrope or azeotrope-like composition consisting essentially of 1-bromopropane and highly fluorinated pentane. The azeotrope solvent composition has a constant boiling point solvent (which does not separate during evaporation or distillation).
a constant boiling solvent). While azeotropes and azeotrope-like compositions are preferred, non-azeotropic compositions comprising 1-bromopropane and highly fluorinated pentane are also considered to be within the scope of the present invention. The use of the solvents prepared according to the present invention cleans various articles having cloth, ceramic, metal, and plucky surfaces.

[0005] For the purposes of the present invention, an azeotropic composition is a composition in which the vapor produced by partial evaporation or partial distillation of a liquid has substantially the same composition as the liquid (ie, the mixture has a composition Distilling without substantial change) is defined as a constant boiling liquid mixture comprising two or more substances that exhibits the physical properties of a single compound. A constant boiling composition (characterized as an azeotrope) exhibits the highest or lowest boiling point compared to the boiling point of a non-azeotropic mixture of the same material. The present invention contemplates, in an azeotrope, a mixture comprising highly fluorinated pentane, 1-bromopentane, and optionally one or more stabilizers and cosolvents.

[0006] By azeotrope-like composition is meant that the composition of the compound has a concentration that is different (but slightly) than that observed in the azeotrope composition. Therefore, the highly fluorinated pentane, 1-, contained in the azeotrope-like composition
The concentrations of bromopropane, and the stabilizers and co-solvents added, may be somewhat different from those observed in the azeotrope formed between them, and remain compositions within the scope of the present invention. It may be. The boiling point of an azeotrope-like composition will be substantially the same as the boiling point of the corresponding azeotrope. Preferably, the azeotrope-like composition boils at ambient pressure and at a temperature within about 2 ° C of the temperature at which the corresponding azeotrope boils at that same pressure.

In addition, when fractional distillation is performed, the concentration of the highly fluorinated pentane, 1-bromopropane, and the added stabilizer and co-solvent is less than the concentration of the azeotrope or azeotrope-like composition. Compositions comprising, at different times, highly fluorinated pentane, 1-bromopropane, and added stabilizers and cosolvents, which result in a distillate that is an azeotrope or azeotrope-like composition, are also provided by the invention Within range. The concentration of the highly fluorinated pentane, 1-bromopropane, and the added stabilizer and co-solvent in such a composition may be about 1% less than the concentration of the azeotrope or azeotrope-like composition.
Preferably, the difference is about 0% by weight or less, and more preferably, about 5% by weight or less.

[0008] By solvating ability is meant the property of a composition in a liquid state that dissolves a solid or semi-solid substance and becomes miscible with liquids, including gums, greases, and gels. At the molecular level, solvation means dispersing material molecules with solvent molecules. It is not necessary that dissolution and miscibility be complete (ie, infinitely soluble or miscible with the substance). However, it goes without saying that the substrate (
By increasing the amount of solvent composition added to the substrate), or by increasing the amount of solvent composition by repeatedly adding essentially uncontaminated solvent, with increasing amounts of solvent or essentially More substance is dissolved sequentially with each successive addition of uncontaminated solvent. One method for evaluating the solvating ability of a solvent is described in ASTM D1133-94 Standard.
The Kauri-Butanol value described in "Test Method for Kauri Butanol Value of Hydrocarbon Solvents" is measured.

[0009] The solvent composition of the present invention comprises a highly fluorinated pentane. The highly fluorinated pentane is preferably decafluoropentane having a boiling point of 55 ° C. at atmospheric pressure.
More preferably, the decafluoropentane consists essentially of 1,1,1,1,2,3,4,4,5,5,5-decafluoropentane. This decafluoropentane is commercially available from DuPont under the trade name Vertrel XF. The solvent composition of the present invention consists essentially of about 84.7% by weight of 1,1,1,2,3,4,4,5,5,5-decafluoropentane and about 15.3% by weight of 1 It is preferably an azeotrope composition consisting of bromopropane and having a boiling point at atmospheric pressure of about 49.2 ° C.

[0010] The solvent composition of the present invention further comprises 1-bromopropane (commercially available from Great Lakes Chemical Corporation). This halogenated solvent has a low boiling point and is inexpensive, and is less harmful to the atmospheric ozone layer than chlorofluorocarbon.
Importantly, 1-bromopropane is non-toxic unlike many other halogenated alkanes. For example, 2-bromopropane is considered to be quite toxic to both humans and animals. 1-bromopropane further comprises
It has a very high solvation capacity as indicated by a Kauri-butanol value of 125.

Although 1-bromopropane is an excellent cleaning solvent for metal parts, its high solvating ability limits its application to plastics and elastomers. 1
-Bromopropane has a tendency to erode or partially dissolve the surface of the latch. A mixture of 1-bromopropane and a less aggressive solvent (e.g., hydrochlorofluorocarbon) reduces the adverse effects on plastics and elastomers while increasing the solvating ability of the hydrochlorofluorocarbon. Finally, the described solvent blends are extremely effective in cleaning a variety of articles having metal, ceramic, fabric, and plastic surfaces.

Although the solvent composition of the present invention contains decafluoropentane and 1-bromopropane at concentrations other than the concentration of the azeotropic mixture, fractional distillation of these solvent compositions gives an azeotropic mixture composition. . The concentration of decafluoropentane and 1-bromopropane is
Preferably the concentration differs from the azeotrope or azeotrope-like composition by no more than about 10% by weight, more preferably no more than about 5% by weight.

[0013] Solvent compositions that do not give an azeotrope composition upon distillation are also included in the present invention. Non-azeotropic solvent compositions are useful for certain applications where separation of the cleaning solvent is not a major concern. The non-azeotropic solvent composition comprises 1-bromopropane and about 1% to about 99% by weight of a highly fluorinated pentane (preferably about 10% to
About 90% by weight, more preferably about 30% to about 70% by weight of highly fluorinated pentane).

[0014] Mixtures of 1-bromopropane and highly fluorinated pentanes result in solvent compositions with high solvating capabilities. By properly selecting the solvent composition, 1-
Cleaning solutions can be prepared that have a lower solvating capacity than bromopropane but higher than highly fluorinated pentane. The solvent of the present invention comprises from about 1% to about 9% by weight.
9% (preferably about 10% to about 90%, more preferably about 30% to about 70% by weight) of 1-bromopropane. The solvent composition of the present invention comprises from about 6 to about 124 (preferably about 25 to about 105, more preferably about 35 to about 95
A) a cleaning solvent having a Kauri-butanol number of 1).

[0015] The solvent composition of the present invention optionally comprises a stabilizer and a co-solvent. These stabilizers and co-solvents are formulated to modify the physical and chemical properties of the solvent composition.
Stabilizers are added to suppress metal-induced decomposition of halogenated hydrocarbons. Reactive metals (eg, aluminum, magnesium, copper, zinc, iron, titanium, tin, and alloys of these metals) often cause the decomposition of halogenated hydrocarbons (1-bromopropane). In general, these metals cause the hydrolysis and / or dehydrogenation of the alkyl halide to produce metal halides, halide salts, and acids as some of the decomposing species. The production of these decomposed species is detrimental to metal parts. Metal bromides and certain metal salts are formed from metal ions extracted from the metal surface, and hydrobromic acid corrodes the metal, which further exacerbates the problem. Therefore, the added stabilizer stabilizes the halogenated solvent in a liquid state and a vapor state so as not to deteriorate in the presence of these metals, and suppresses the formation of decomposition products of the metal complex and the solvent. Reduces the attack on the metal by certain of these decomposition products. Stabilizers incorporated as optional components of the solvent composition include alcohols, ketones, ethers, acetals, nitroalkanes, epoxides, amines, and mixtures of these stabilizers.

Examples of alcohols that can be added to the solvent include ethyl alcohol, propyl alcohol, isopropyl alcohol, t-butyl alcohol, t-amyl alcohol, sec-butyl alcohol, phenols (for example, phenol,
p-cresol, m-cresol, and o-cresol), amino alcohols (eg, monoethanolamine, diethanolamine, and triethanolamine), acetylenic alcohols (eg, methylbutynol and methylpentinol), benzotriazole, and mixtures of alcohols And the like, but are not limited to these.

Representative ketones useful in the present invention include acetone, methyl ethyl ketone (MEK), 2-propanone (diethyl ketone), 2-pentanone, 3-pentanone, 2-hexanone, 3-hexanone, 2-heptanone, 3 -Heptanone, 4
-Heptanone, 2,6-dimethyl-4-heptanone, 2-methyl-3-heptanone, 2-methyl-2-butanone, 2-methyl-3-pentanone, 2-nonanone,
And mixtures of these ketones.

Specific examples of ethers that can be added to the stabilizing solvent include diethyl ether, dipropyl ether, dibutyl ether, methyl t-butyl ether,
, 4-dioxane, 1,3-dioxane, trioxane, γ-butyrolactone, tetrahydrofuran, dialkyl ethers of ethylene glycol (eg, dimethyl ethylene glycol ether and diethyl ethylene glycol ether), and cellosolve (CELLOSOLVE). , 1-1
Monoalkyl ethylene glycol ethers having zero carbon atoms (eg, methyl cellosolve, ethyl cellosolve, and isopropyl cellosolve) and the like. These ethers are added to the solvent alone or as a mixture of two or more.

Examples of acetals suitable for the present invention include the dimethyl acetal and diethyl acetal of the above ketones. Representative nitroalkanes useful in the present invention include nitromethane, nitroethane, 1-nitropropane, 2-nitropropane, nitrobutane, and mixtures of these nitroalkanes.

Particular examples of epoxides useful in the present invention include epibromohydrin,
Examples include propylene oxide, 1,2-butylene oxide, 2,3-butylene oxide, cyclohexene oxide, glycidyl methyl ether, glycidyl methacrylate, pentene oxide, cyclopentene oxide, and cyclohexene oxide. The epoxide is added to the stabilizing solvent alone or as a mixture of two or more.

Non-nucleophilic amines are preferred, and thus secondary and tertiary amines are desirable. Examples of amines useful for the present invention include hexylamine, octylamine, 2-ethylhexylamine, dodecylamine, ethylbutylamine, hexylmethylamine, butyloctylamine, dibutylamine, octadecylmethylamine, triethylamine, tributylamine, Diethyloctylamine,
Tetradecyldimethylamine, dibutylamine, diisobutylamine, diisopropylamine, pentylamine, N-methylmorpholine, isopropylamine,
Cyclohexylamine, butylamine, isobutylamine, dipropylamine,
2,2,6,6-tetramethylpiperidine, N, N-dimethyl-p-phenylamine, N, N-diethyl-p-phenylamine, diethylamine, aniline, ethylenediamine, propylenediamine, triethylamine, tetraethylenepentamine Benzylamine, dibenzylamine, diphenylamine, and diethylhydroxyamine. These amines are useful alone or in combination of two or more.

Examples of co-solvents include alkanes, alkenes, alkynes, alcohols, ketones, esters, terpenes, and various aliphatic mixtures, including mineral spirits, VM & P naphtha, and Stoddard solvents. Many of the above stabilizers are also thought to be co-solvents. Co-solvents are added to change the solvating capacity of the solvent composition. Thus, for example, by adding alcohol or ketone,
-The ability to solvate bromopropane can be reduced. The co-solvent further imparts a higher degree of polarity and hydrogen bonding properties to the solvent, so that the solvent can effectively remove ionic or polar contaminants. Further, these co-solvents are often less expensive than highly fluorinated pentanes, thus reducing the costs associated with preparing and using solvent blends.

The solvent composition of the present invention is obtained by mixing 1-bromopropane with a sufficient amount of a highly fluorinated pentane to obtain a desired cleaning solvent having a specific concentration or a desired Kauri-butanol value. It is manufactured by doing. The order in which the components are added is not important to the invention. Add stabilizers and cosolvents as needed. Further, a small amount of a surfactant can be added. Representative surfactants useful in the present invention include ionic and non-ionic surfactants, such as sulfonates, phosphates, carboxylates, fatty acids, alkylphenols, glycols, esters, and amides. There is. Surfactants further include ionic and non-ionic water displacement compounds, such as tetraalkylammonium sulfonic acid salts, tetraalkylammonium phosphate salts, tetraalkylammonium carboxylate salts, bromide salts, and the like. Examples include aliphatic aminoalkanols, fluorinated aminoalkanols, and fluorinated aminoalkanols. Again, the order of addition is not important to the invention.

[0024] The solvent composition of the present invention is suitable for cleaning articles having cloth, metal, ceramic, plastic, and elastomeric surfaces. Solvent composition of the present invention,
It can be applied by any known method or by any of the methods commonly used to clean or degrease articles. For example, the surface of the article may be wiped with an absorbent medium containing the solvent composition (eg, a cloth saturated with a solvent). The article may be immersed or partially immersed in the immersion tank. The solvent in the immersion tank can be hot or cold, and the article can be immersed for a long time without causing solvent degradation. Furthermore, the articles, dip tanks and related parts are not harmed by this process. Alternatively, a solvent may be sprayed onto the article, or the article may be cleaned in a vapor degreasing chamber using a liquid or vaporized solvent composition.

When the solvent is applied as a vapor, the solvent is generally vaporized by heating the solvent in a solvent reservoir. The vaporized solvent then condenses on the surface of the article. The condensed solvent solvates or entrains grease, oils, contaminants, and other undesirable particles present on the surface of the article. The contaminated solvent flows away into the solvent reservoir, thus dissolving and entrained material is carried to the reservoir. As only the solvent is vaporized, grease, oil, and contaminants remain in the reservoir, and the article is continuously washed away with clean solvent.

Hereinafter, the present invention will be described in more detail with reference to examples, but the present invention is not limited to these examples. Embodiment 1 FIG. Gas for azeotrope composition 1-bromopropane and decafluoropentane containing decafluoropentane and 1-bromopropane - liquid diagram was determined by mixing the solvent at various concentrations. The solvent composition was distilled in a 100 ml Osmer still. The solvent was heated to reflux to equilibrate. Samples of the vapor portion and the liquid portion were collected and analyzed using a gas chromatograph to determine the concentration of the components. The results obtained are shown in Table 1 and are shown graphically in FIG.
By analyzing the obtained results, 1-bromopropane and 1,1,1,2,3,4,
It was found that an azeotrope composition consisting of 4,5,5,5-decafluoropentane was present.

[0027]

[Table 1]

Based on these initial results, about 81.2% by weight of 1,1,1,2,3,4,4,5,5,5-decafluoropentane and about 17.8% by weight of 1 A second solvent composition consisting of -bromopropane was prepared. This second solvent mixture was distilled in a Perkin Elmer model 151 annular still (200 theoretical plates capacity). After the refluxing solvent was in equilibrium, a distillate fraction comprising about 10% by weight of the total liquid charge was collected at a reflux to extract ratio of 10: 1. The boiling point of each fraction was measured to the 0.1 ° C scale. 1-bromopropane and 1,1,1,2,3,4,4,
The concentration of the 5,5,5-decafluoropentane fraction was determined using a gas chromatograph. Table 2 shows the result of the second distillation. By analyzing the results described in Table 2, about 15.3% by weight of 1-bromopropane and about 84.7% by weight
Confirmed that an azeotropic mixture consisting of 1,1,1,1,2,3,4,4,5,5,5-decafluoropentane exists and that the azeotropic mixture boils at about 80.2 ° C Is done.

[0029]

[Table 2]

Embodiment 2 FIG . About 33% by weight of a solvent composition containing 1,1,1,2,3,4,4,5,5,5-decafluoropentane, 1 -bromopropane, and isopropyl alcohol is 1,1,1,2, A solvent composition was prepared comprising 3,4,4,5,5,5-decafluoropentane, about 33% by weight of 1-bromopropane, and about 33% by weight of isopropyl alcohol. As an initial screening evaluation, 100 g of this solvent mixture was distilled on a Perkin Elmer Annular Distiller Model 151 (200 theoretical plates capacity). The solvent was heated to reflux to equilibrate. Three distillate fractions were collected at a reflux to extract ratio of 10: 1. The concentration of 1,1,1,1,2,3,4,4,5,5,5-decafluoropentane and isopropyl alcohol was measured for each fraction using a gas chromatograph. Table 3 shows the obtained results. By analyzing the results, it can be seen that the solvent composition is separated during the distillation. Despite the separation, this solvent composition performs well as a cleaning and degreasing solvent in applications where separation of the solvent is not critical.

[0031]

[Table 3]

Embodiment 3 FIG . 1-bromopropane and 1,1,1,2,3,4,4,5,5,5 Dekafu Ruoropentan and containing methanol azeotrope composition like the weight of 1-bromopropane and 1,1,1 , 2,3,4,4,5,5,5-Decafluoropentane and a solvent composition containing methanol were prepared. This solvent composition 100
g was distilled in a Perkin Elmer still 151 model 200 (200 theoretical plates capacity). The solvent mixture was heated to reflux and brought to equilibrium before collecting three 10 g fractions. For each fraction, the concentrations of 1,1,1,1,2,3,4,4,5,5,5-decafluoropentane, 1-bromopropane, and methanol were measured using a gas chromatograph. Very little separation was observed in this pre-distillation. Based on the results of this initial distillation, 82% by weight of 1,1,1,2,3,4,4,5,
A second solvent composition was prepared containing 5,5-decafluoropentane, 5.6% by weight methanol, and 16.1% by weight 1-bromopropane. This second solvent composition was distilled as described above. Distillate fraction (each about 1% of total solvent weight)
0% by weight) was collected at a reflux to extract ratio of 10: 1. The composition of the distillate fraction was analyzed using a gas chromatograph. Table 4 shows the composition data and boiling point of the distillate. Analysis of the results described in Table 4 confirms that very little separation occurs between the three components during distillation and that an azeotrope is present. The azeotrope consists essentially of about 80.8% by weight of 1,1,1,2,3,4,4,5,5,5-decafluoropentane, about 5.7% by weight of methanol, and It consists of about 13.6% by weight of 1-bromopropane and has a boiling point of about 50 ° C.

[0033]

[Table 4]

Embodiment 4 FIG . 1,1,1,2,3,4,4,5,5,5-decafluoropentane, an azeotrope composition comprising 1 -bromopropane and acetone , 1,1,1,1,2,3, A solvent composition containing 4,4,5,5,5-decafluoropentane, 1-bromopropane and acetone was prepared. To first determine whether these three components form an azeotrope composition, the resulting solution was fractionally distilled on a Perkin Elmer Annular Still Still Model 151 as described in Example 2. did. Based on the results of this initial evaluation, about 32.5% by weight of 1,1,1,2,3,4,4,5,5,5-decafluoropentane, 29.9% by weight of 1- A second solvent blend containing bromopropane and about 37.4% by weight acetone was prepared. This second solvent composition was fractionally distilled using a Perkin Elmer still. After heating the solvent to reflux and equilibrating, a distillate fraction of about 10% by weight, based on the total weight of the solvent, was collected at a reflux to extract ratio of 10: 1. Each distillate fraction was analyzed by gas chromatography to determine the concentration of each component. Table 5 shows the obtained results.

[0035]

[Table 5]

Embodiment 5 FIG . About 33% by weight of a solvent blend containing 1,1,1,1,2,3,4,4,5,5,5-decafluoropentane, 1 -bromopropane and nitropropane in 1,1,1,2,3 A solvent composition comprising 1,4,4,5,5,5-decafluoropentane, about 33% by weight of 1-bromopropane and about 33% by weight of butylene oxide was prepared, as described in Example 2. Distilled. Table 6 shows the results of the distillation.

[0037]

[Table 6]

According to an analysis of the results obtained, it is found that the composition contains approximately equal weights of 1,1,1,2,3,4,4,5,5,5-decafluoropentane, 1-bromopropane and nitromethane. It is not confirmed that an azeotrope composition exists for the solvent composition. However, this solvent mixture is an excellent cleaning and degreasing solvent for operations where separation is not important.

Embodiment 6 FIG . About 32% by weight of a solvent blend containing 1,1,1,1,2,3,4,4,5,5,5-decafluoropentane, 1 -bromopropane, isopropyl alcohol and nitromethane , 1,1,1,2 Preparing a solvent composition comprising, 3,4,4,5,5,5-decafluoropentane, about 32% by weight of 1-bromopropane, about 32% by weight of isopropyl alcohol and about 4% by weight of nitromethane; Distilled as described in Example 2. Table 7 shows the results of the distillation.

[0040]

[Table 7]

According to the analysis of the obtained results, it was found that approximately equal weights of 1,1,1,2,3,4,4,5,5,5-decafluoropentane, 1-bromopropane, isopropyl alcohol and 4
No azeotrope composition is found to exist for the solvent composition containing nitromethane by weight. This solvent mixture is an excellent cleaning and degreasing solvent for operations where separation is not important.

[Brief description of the drawings]

FIG. 1 shows 1,1,1,1,2,3,4,4,5,5,5-decafluoropentane in a composition in a liquid phase and a gaseous phase obtained during distillation of a solvent composition. Are plotted.

[Procedure amendment]

[Submission date] January 17, 2000 (2000.1.17)

[Procedure amendment 1]

[Document name to be amended] Statement

[Correction target item name] Claims

[Correction method] Change

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[Claims]

[Procedure amendment 2]

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Embodiment 3 FIG . 1-bromopropane and 1,1,1,2,3,4,4,5,5,5 Dekafuru Oropentan and containing methanol azeotrope composition like the weight of 1-bromopropane and 1,1,1 , 2,3,4,4,5,5,5-Decafluoropentane and a solvent composition containing methanol were prepared. This solvent composition 100
g was distilled in a Perkin Elmer still 151 model 200 (200 theoretical plates capacity). The solvent mixture was heated to reflux and brought to equilibrium before collecting three 10 g fractions. For each fraction, the concentrations of 1,1,1,1,2,3,4,4,5,5,5-decafluoropentane, 1-bromopropane, and methanol were measured using a gas chromatograph. Very little separation was observed in this pre-distillation. Based on the results of the initial distillation, a second solvent composition was prepared. This second
Was distilled as described above. Distillate fractions (each about 10% by weight of total solvent weight) were collected at a 10: 1 reflux to extract ratio. The composition of the distillate fraction was analyzed using a gas chromatograph. Table 4 shows the composition data and boiling point of the distillate. Analysis of the results described in Table 4 confirms that very little separation occurs between the three components during distillation and that an azeotrope is present. This azeotrope is essentially about 80.8% by weight of 1.1
, 1,2,3,4,4,5,5,5-decafluoropentane, about 5.7% by weight of methanol, and about 13.6% by weight of 1-bromopropane at a temperature of about 50 ° C. It has a boiling point.

[Procedure amendment 3]

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[0033]

[Table 4]

[Procedure amendment 4]

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Embodiment 5 FIG . 1,1,1,2,3,4,4,5,5,5-decafluoropentane and 1-Bed Romopuropan and solvent blend of about 33 wt% of 1,1,1,2,3 containing a nitromethane, A solvent composition comprising 4,4,5,5,5-decafluoropentane, about 33% by weight of 1-bromopropane and about 33% by weight of nitromethane was prepared and distilled as described in Example 2. .

[Procedure amendment 5]

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[Correction method] Deleted

[Procedure amendment]

[Submission date] October 25, 2000 (2000.10.25)

[Procedure amendment 1]

[Document name to be amended] Drawing

[Correction target item name] All figures

[Correction method] Change

[Correction contents]

FIG.

──────────────────────────────────────────────────続 き Continuation of front page (81) Designated country EP (AT, BE, CH, CY, DE, DK, ES, FI, FR, GB, GR, IE, IT, LU, MC, NL, PT, SE ), OA (BF, BJ, CF, CG, CI, CM, GA, GN, GW, ML, MR, NE, SN, TD, TG), AP (GH, GM, KE, LS, MW, SD, SZ, UG, ZW), EA (AM, AZ, BY, KG, KZ, MD, RU, TJ, TM), AL, AM, AT, AU, AZ, BA, BB, BG, BR, BY, CA, CH, CN, CU, CZ, DE, DK, EE, ES, FI, GB, GE, GH, GM, HR, HU, ID, IL, IS, JP, KE, KG, KP , KR, KZ, LC, LK, LR, LS, LT, LU, LV, MD, MG, MK, MN, MW, MX, NO, NZ, PL, PT, RO, RU, SD, SE, SG, SI, SK, SL, TJ, TM, TR, TT, UA, UG, US, UZ, VN, YU, ZW (71) Applicant Post Office Box 2200, Highway 52N. W. , West Lafayette, Indiana 47906, United States of America F-term (reference) 4H003 DA12 DA14 DA15 ED26 ED27 ED28 ED29 ED30 ED31 FA46 4K053 PA01 QA04 RA33 RA36 RA40 SA02 SA03 SA06

Claims (22)

[Claims] 1 to about 99% by weight of a hydrofluorocarbon and 1-bromo acid consisting essentially of 1,1,1,1,2,3,4,4,5,5,5-decafluoropentane. A solvent composition comprising propane. 2. The composition of claim 1, comprising from about 10% to about 90% by weight of said hydrofluorocarbon. 3. The composition of claim 2, comprising from about 30% to about 70% by weight of said hydrofluorocarbon. 4. The composition of claim 1, comprising an azeotrope or azeotrope-like composition of 1-bromopropane and said hydrofluorocarbon. 5. The composition according to claim 1, consisting essentially of 1-bromopropane and a hydrofluorocarbon, which, when fractionated, results in a fractionated distillate that is an azeotrope or an azeotrope-like composition. The composition of claim 1, wherein the concentration of 1-bromopropane and hydrofluorocarbon at this time differs from the concentration of the azeotrope or azeotrope-like composition by about 10% by weight or less. 6. About 11% to about 17% by weight of 1-bromopropane and about 83% by weight.
The composition of claim 1, comprising from about 90% to about 90% by weight of the hydrofluorocarbon. 7. The composition of claim 1, having a Kauri-butanol value of about 5 to about 125.
A composition as described. 8. The composition according to claim 1, further comprising a stabilizer selected from the group consisting of alcohols, ketones, nitroalkanes, epoxides, amines, ethers, and mixtures thereof. 9. The composition according to claim 8, wherein said stabilizer is a C ₁ -C ₅ alcohol. 10. The composition of claim 9, comprising a ternary or ternary azeotrope-like composition of 1-bromopropane, said hydrofluorocarbon, and said alcohol. 11. The process of claim 9 wherein said fractional distillation consists essentially of 1-bromopropane, said hydrofluorocarbon, and said alcohol, which upon distillation yields a fractional distillate that is an azeotrope or azeotrope-like composition. A composition of
10. The composition according to claim 9, wherein the concentration of 1-bromopropane, hydrofluorocarbon and alcohol differs from the concentration of the azeotrope or azeotrope-like composition by about 10% by weight or less. 12. About 12% to about 16% by weight of 1-bromopropane, about 7% by weight.
10. The composition of claim 9, comprising from 8% to about 84% by weight of the hydrofluorocarbon, and from about 5% to about 6% by weight of methanol. 13. About 20% to about 25% by weight of 1-bromopropane, about 7% by weight.
10. The composition of claim 9, comprising from 0% to about 80% by weight of the hydrofluorocarbon, and from about 1% to about 5% by weight of 2-propanol. 14. The composition of claim 8, wherein said stabilizer is a ketone. 15. The azeotropic or ternary azeotrope-like composition of 1-bromopropane, the hydrofluorocarbon, and the ketone.
4. The composition according to 4. 16. The process of claim 14 wherein said fractional distillation consists essentially of 1-bromopropane, said hydrofluorocarbon, and said ketone, resulting in a fractionated distillate that is an azeotrope or azeotrope-like composition. 15. The composition of claim 14, wherein the concentrations of 1-bromopropane, hydrofluorocarbon and ketone differ from the concentration of the azeotrope or azeotrope-like composition by about 10% by weight or less. Composition. 17. About 24% to about 31% by weight of 1-bromopropane, about 2% to about 31% by weight.
6% to about 35% by weight hydrofluorocarbon, and about 35% to about 4%
The composition according to claim 14, comprising 6% by weight of acetone. 18. About 15% to about 25% by weight of 1-bromopropane, about 6% by weight.
5% to about 75% by weight hydrofluorocarbon, and about 5% to about 15%
9. The composition of claim 8, wherein the composition comprises by weight butylene oxide. 19. The method of claim 1, wherein the hydrofluorocarbon and 1-bromopropane consist essentially of 1,1,1,2,3,4,4,5,5,5-decafluoropentane. A method for cleaning an article, comprising the step of contacting the article with a solvent composition comprising: 20. The method of claim 16, wherein the solvent composition comprises from about 10% to about 90% by weight of the hydrofluorocarbon. 21. The cleaning method of claim 17, wherein said solvent composition comprises from about 30% to about 70% by weight hydrofluorocarbon. 22. The cleaning method of claim 16, wherein said solvent composition further comprises a stabilizer selected from the group consisting of alcohols, ketones, nitroalkanes, epoxides, amines, ethers, and mixtures thereof.