Patent Publication Number: US-6042749-A

Title: Mixed solvent composition

Description:
This application is a Continuation Division Continuation-in-part (CIP) of application Ser. No. 08/578,533, now U.S. Pat. No. 5,827,454 filed on Jan. 18, 1996 which was filed as International Application PCT/JP95/00948 on May 18, 1995. 
    
    
     BACKGROUND OF THE INVENTION 
     1. Field of the Invention 
     The present invention relates to mixed solvent compositions used as cleaning agents for electronic components including a printed circuit board and an IC, precision machinery parts, of glass substrates, for example. 
     Abbreviations and terms used in the present specification are illustrated below. 
     R113: 1,1,2-trichloro-1,2,2-trifluoroethane 
     R225; a mixture of one or two or more of dichloropentafluoropropane having the molecular formula C 3  HCl 2  F 5   
     R225ca: 3,3-dichloro-1,1,1,2,2-pentafluoropropane 
     R225cb: 1,3-dichloro-1,1,2,2,3-pentafluoropropane 
     R225mix: a mixture of at least two dichloropentafluoropropane isomers selected from the group consisting of R225ca, R225cb and other dichloropentafluoropropane isomers 
     R43-10mee: 1,1,1,2,3,4,4,5,5,5-decafluoropentane R51-14M: a mixture of one or two or more of perfluorohexane having the molecular formula C 6  F 14   
     R51-14: perfluoro (n-hexane) 
     R51-14my: perfluoro (4-methylpentane) 
     R51-14mcy: pefluoro (3-methylpentane) 
     R51-14mix: a mixture of at least two perfluorohexane isomers selected from the group consisting of R51-14, R51-14my, R51-14mcy and other perfluorohexane isomers 
     Azeotropic mixed solvent composition: a mixed solvent composition, the composition of which does not substantially vary even by repeating distillation-condensation operations 
     Azeotropic-like mixed solvent composition: a mixed solvent composition, the composition of which varies only within the range of ±2% even by repeating distillation-condensation operations 
     2. Description of the Background 
     To remove various oils, greases, or fluxes for example, R113 which is nonflammable, low toxic and excellent in stability, or a mixed solvent composition comprising R113 and a solvent miscible with R113 is widely used. Since R113 has such characteristics that it does not have an adverse effect on a base material such as a metal, a plastic or an elastomer and selectively dissolves various soils, it has been suitable for cleaning various electronic components, precision machinery parts, or components for example, made of a metal, a plastic, or an elastomer for example. Also, U.S. Pat. No. 5,304,322 discloses a cleaning agent for aircrafts, which comprises a C 4  -C 8  perfluorocarbon, a C 2  -C 5  hydrochlorofluorocarbon and a C 5  -C 9  petroleum distillate. In spite of various advantages of conventionally used R113, its production and consumption are regulated, because it has such a long life time in the troposphere by virtue of its chemical stability that it can diffuse to the stratosphere, where it is decomposed by an ultraviolet ray, producing chlorine radicals and the chlorine radicals cause a chain reaction with stratospheric ozone to deplete the ozone layer. 
     For this reason, alternative solvents to R113, which do not cause depletion of the ozone layer are widely being researched. 
     An object of the present invention is to provide a novel mixed solvent composition which satisfies the excellent properties of conventional R113 and can be used as an alternative solvent which does not substantially affect the ozone layer. 
     DISCLOSURE OF INVENTION 
     The present invention has been made to accomplish the above object, and provides a mixed solvent composition which comprises R225 and at least one component selected from the group consisting of R43-10mee and R51-14M, as the essential components, and a mixed solvent composition which comprises R225, an alcohol and at least one component selected from the group consisting of R43-10mee and R51-14M. In the following description including Examples, &#34;%&#34; means &#34;% by weight&#34;. 
     In the mixed solvent composition comprising R225 and at least one of R43-10mee and R51-14M, as the essential components, the proportion of each of R43-10mee and R51-14M is preferably from 10 to 1,000 parts by weight to 100 parts by weight of R225. More preferable examples include the following azeotoropic or azeotropic-like mixed solvent compositions (1) to (13). 
     (1) An azeotropic-like mixed solvent composition comprising from 40 to 55% of R43-10mee and from 45 to 60% of R225ca. 
     (2) An azeotropic mixed solvent composition comprising 48% of R43-10mee and 52% of R225ca. 
     (3) An azeotropic-like mixed solvent composition comprising from 50 to 70% of R43-10mee and from 30 to 50% of R225cb. 
     (4) An azeotropic mixed solvent composition comprising 58% of R43-10mee and 42% of R225cb. 
     (5) An azeotropic-like mixed solvent composition comprising from 10 to 50% of R225mix and from 50 to 90% of R43-10mee. 
     (6) An azeotropic-like mixed solvent composition comprising from 30 to 75% of R225ca and from 25 to 70% of R51-14mix comprising R51-14 as the main component. 
     (7) An azeotropic-like mixed solvent composition comprising from 30 to 75% of R225ca and from 25 to 70% of R51-14. 
     (8) An azeotropic mixed solvent composition comprising 55% of R225ca and 45% of R51-14. 
     (9) An azeotropic-like mixed solvent composition comprising from 25 to 60% of R225cb and from 40 to 75% of R51-14mix comprising R51-14 as the main component. 
     (10) An azeotropic-like mixed solvent composition comprising from 25 to 60% of R225cb and from 40 to 75% of R51-14. 
     (11) An azeotropic mixed solvent composition comprising 45% of R225cb and 55% of R51-14. 
     (12) An azeotropic-like mixed solvent composition comprising from 25 to 70% of R225mix and from 30 to 75% of R51-14mix comprising R51-14 as the main component. 
     (13) An azeotropic-like mixed solvent composition comprising from 25 to 70% of R225mix and from 30 to 75% of R51-14. 
     The present invention further provides a mixed solvent composition comprising R225, an alcohol and at least one component selected from the group consisting of R43-10mee and R51-14M, as the essential components. Preferably, in this composition, the proportion of R43-10mee is from 10 to 1000 parts by weight, the proportion of R51-14M is from 30 to 500 parts by weight and the proportion of an alcohol is from 1 to 100 parts by weight, to 100 parts by weight of R225. More preferable examples include the following azeotrophic or azeotrophic-like mixed solvent compositions (14) to (16). 
     (14) An azeotropic-like mixed solvent composition comprising from 20 to 50% of R225mix, from 45 to 75% of R51-14M and from 3 to 10% of methanol. 
     (15) An azeotropic-like mixed solvent composition comprising from 20 to 45% of R225mix, from 47 to 75% of R51-14M and from 3 to 8% of ethanol. 
     (16) An azeotropic-like mixed solvent composition comprising from 20 to 60% of R225mix, from 38.5 to 75% of R51-14M and from 1.5 to 7% of 2-propanol. 
     In addition to the above-mentioned methanol, ethanol and 2-propanol, preferable other examples of an alcohol include 1-propanol, 1-buthanol, 2-buthanol, isobuthanol, t-buthanol and the like. 
     Preferable examples of R225 include R225ca or R225cb respectively alone or a mixture of R225ca and R225cb. The mixture of R225ca and R225cb is preferably a mixture of from 0.01 to 99.99% of R225ca and from 0.01 to 99.99% of R225cb, more preferably a mixture of from 1 to 99% of R225ca and from 1 to 99% of R225cb. The mixture of R225ca and R225cb exhibits azeotropic-like action in a wide composition range. A preferable example of R225mix include a mixture of R225ca and R225cb. 
     R51-14M is preferably R51-14, R51-14my or R51-14mcy respectively alone or a mixture of at least one of these compounds. When R51-14M is a mixture, such a mixture should preferably comprise R51-14 as the main component. A preferable mixture example of R51-14M is a mixture comprising from 65 to 77% of R51-14, from 16 to 26% of R51-14my and from 2 to 12% of R51-14mcy, more preferably a mixture comprising from 70 to 75% of R51-14, from 18 to 22% of R51-14my and from 5 to 10% of R51-14mcy. 
     In order to improve mainly a dissolving property, the mixed solvent composition of the present invention may contain one or two or more compounds selected from the following compounds in an amount of from 0.1 to 50%, preferably from 0.1 to 30%, more preferably from 0.1 to 20%: 
     hydrocarbons such as n-pentane, 2-methylbutane, 2,2-dimethylpropane, n-hexane, 3-methylpentane, 2,2-dimethylbutane, 2,3-dimethylbutane, n-heptane, 2-methylhexane, 3-methylhexane, 2,3-dimethylpentane, 2,4-dimethylpentane, n-octane, 2,2,3-trimethylpentane, 2,2,4-trimethylpentane, cyclopentane, cyclohexane, methylcyclohexane and ethylcyclohexane; 
     chlorinated hydrocarbons such as dichloromethane cis-1,2-dichloroethylene, trans-1,2-dichloroethylene, trichloroethylene and tetrachloroethylene; 
     ketones such as acetone, methyl ethyl ketone, methyl butyl ketone and methyl isobutyl ketone; 
     ethers such as diethyl ether, methyl cellosolve, tetrahydrofuran and 1,4-dioxane; 
     chlorofluorohydrocarbons such as 2,2-dichloro-1,1,1-trifluoroethane and 1,1-dichloro1-fluoroethane; and 
     esters such as methyl acetate, ethyl acetate, propyl acetate and butyl acetate. 
     In order to improve mainly a stability, the mixed solvent composition of the present invention may contain one or two or more compounds selected from the following compounds in an amount of from 0.001 to 10%, preferably from 0.001 to 5%: 
     nitro compounds such as nitromethane, nitroethane, nitropropane and nitrobenzene; 
     amines such as diethylamine, triethylamine, i-propylamine, n-butylamine and i-butylamine; 
     phenols such as phenol, o-cresol, m-cresol, p-cresol, thymol, p-t-butylphenol, t-butylcatechol, catechol, isoeugenol, o-methoxyphenol, bisphenol A, isoamyl salicylate, benzyl salicylate, methyl salicylate and 2,6-di-t-butyl-p-cresol; and 
     triazoles such as 2-(2&#39;-hydroxy-5&#39;-methyl-phenyl)benzotriazole, 2-(2&#39;-hydroxy-3&#39;-t-buthyl-5&#39;-methylphenyl)-5-chlorobenzotriazole, 1,2,3-benzotriazole and 1-[(N,N-bis-2-ethylhexyl)aminomethyl]benzotriazole. 
     The mixed solvent composition of the present invention has a dissolving power at the same degree as a conventional R113 type solvent, and can be used suitably in various ways. Specifically, it is used as a paint solvent, an extractant, or a cleaning agent for removing grease, oil, wax, ink or the like. Also, it is used as a cleaning agent or a dust-removing agent for glass, ceramic, plastic, elastomer, rubber, metal or other various articles. More specifically, it is used suitably as a cleaning agent or a dust-removing agent for ICs, electric devices, precision machines, optical lenses or the like. 
     As a cleaning method, various methods including manual wiping, immersing, spraying, vibrating, supersonic cleaning, vapor degreasing or a combination of these methods, may be used. 
     The mixed solvent composition of the present invention provides the excellent properties of conventional R113 and also provides an advantage that it does not substantially affect the ozone layer. 
    
    
     BEST MODE FOR CARRYING OUT THE INVENTION 
     The present invention is further illustrated by the following Examples. 
     Evaluation was conducted by the following three methods. 
     (1) A test coupon (25 mm×30 mm×2 mm) made of SUS-304 was dipped in a machine oil (CQ-30, manufactured by Nippon Petrochemicals Co., Ltd.) and then immersed in the mixed solvent compositions of the present invention as identified in Tables for 5 minutes. Thereafter, the degree of removal of the machine oil was evaluated. The results are shown with evaluation standards for the degree of removal A such that ⊚: excellently removed, Δ: slightly remained and X: substantially remained. 
     (2) Flux (speedy flux AGF-J-I: manufactured by Asahi Kagaku Kenkyusho) was coated on the entire surface of a printed circuit board (50 mm×100 mm×1.6 mm) made of epoxy-glass, and soldering was carried out at a soldering temperature of 260° C. by means of a wave soldering machine. Then, defluxing was carried out by immersing it in the compositions of the present invention as identified in Tables for 3 minutes, and the degree of removal of the flux was evaluated. The results are shown with evaluation standards for the degree of removal B such that ⊚: excellently removed, Δ: slightly remained and X: substantially remained. 
     (3) A glass plate of 30 mm×18 mm×5 mm in size was dipped in pure water and then immersed in the compositions of the present invention shown in Tables for 20 seconds to be dewatered. The glass plate was taken out and immersed in anhydrous methanol, and the degree of removal of deposited water was evaluated from the increase of water in the methanol. The results are shown with evaluation standards for the degree of removal C such that ⊚: excellently removed, Δ: slightly remained and X: substantially remained. 
     EXAMPLE 1 
     1,000 g of a mixed solvent composition consisting of 48% of R43-10mee (b.p. 53.6° C.) and 52% of R225ca (b.p. 51.1° C.) was charged into a distillation flask, and the flask was connected to a distillation column having a number of theoretical plates of 5. Then, the composition was heated and refluxed for 2 hours. After the composition reached equilibrium, the fraction was periodically collected and analyzed by gas chromatography. The results are shown in Table 1. 
     
                       TABLE 1                                                     
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Portion of fraction                                                       
                 Composition (%)                                          
collected (%)    R43-10mee R225ca                                         
______________________________________                                    
20               48.0      52.0                                           
  40 48.0 52.0                                                            
  60 48.0 52.0                                                            
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     EXAMPLE 2 
     20 kg of mixed solvent composition consisting of 55% of R43-10mee and 45% of R225ca was charged into a small degreaser with one-sump, and the degreaser was operated for 6 hours per day for 3 days. Samples were periodically taken from the cleaning sump and the water separator and analyzed by gas chromatography. The results are shown in Table 2. 
     
                       TABLE 2                                                     
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       Composition (%)                                                    
         Cleaning sump   Water separator                                  
Time     R43-10mee  R225ca   R43-10mee                                    
                                      R225ca                              
______________________________________                                    
After 6 hours                                                             
         55.0       45.0     55.0     45.0                                
  After 12 hours 55.1 44.9 55.0 45.0                                      
  After 18 hours 55.1 44.9 54.9 45.1                                      
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     EXAMPLE 3 
     The same procedure as in Example 2 was repeated, except that 20 kg of a mixed solvent composition consisting of 40% of R43-10mee and 60% of R225ca was used as a mixed solvent composition. The results are shown in Table 3. 
     
                       TABLE 3                                                     
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       Composition (%)                                                    
         Cleaning sump   Water separator                                  
Time     R43-10mee  R225ca   R43-10mee                                    
                                      R225ca                              
______________________________________                                    
After 6 hours                                                             
         40.0       60.0     40.0     60.0                                
  After 12 hours 39.9 60.1 40.1 59.9                                      
  After 18 hours 39.9 60.1 40.1 59.9                                      
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     EXAMPLE 4 
     The same procedure as in Example 1 was repeated, except that 1,000 g of a mixed solvent composition consisting of 58% of R43-10mee and 42% of R225cb (b.p. used as a mixed solvent composition. The shown in Table 4. 
     
                       TABLE 4                                                     
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Portion of fraction                                                       
                 Composition (%)                                          
collected (%)    R43-10mee R225cb                                         
______________________________________                                    
20               58.0      42.0                                           
  40 58.0 42.0                                                            
  60 58.0 42.0                                                            
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     EXAMPLE 5 
     The same procedure as in Example 2 was repeated, except that 20 kg of a mixed solvent composition consisting of 70% of R43-10mee and 30% of R225cb was used as a mixed solvent composition. The results are shown in Table 5. 
     
                       TABLE 5                                                     
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       Composition (%)                                                    
         Cleaning sump   Water separator                                  
Time     R43-10mee  R225cb   R43-10mee                                    
                                      R225cb                              
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After 6 hours                                                             
         70.0       30.0     70.0     30.0                                
  After 12 hours 70.1 29.9 70.0 30.0                                      
  After 18 hours 70.1 29.9 69.9 30.1                                      
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     EXAMPLE 6 
     The same procedure as in Example 2 was repeated, except that 20 kg of a mixed solvent composition consisting of 50% of R43-10mee and 50% of R225cb was used as a mixed solvent composition. The results are shown in Table 6. 
     
                       TABLE 6                                                     
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       Composition (%)                                                    
         Cleaning sump   Water separator                                  
Time     R43-10mee  R225cb   R43-10mee                                    
                                      R225cb                              
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After 6 hours                                                             
         50.0       50.0     50.0     50.0                                
  After 12 hours 49.9 50.1 50.1 49.9                                      
  After 18 hours 49.9 50.1 50.1 49.9                                      
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     EXAMPLE 7 
     The same procedure as in Example 2 was repeated, except that 20 kg of a mixed solvent composition consisting of 90% of R43-10mee and 10% of R225mix (R225ca/R225cb=45%/55% mixture) was used as a mixed solvent composition. The results are shown in Table 7. 
     
                       TABLE 7                                                     
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       Composition (%)                                                    
         Cleaning sump   Water separator                                  
Time     R43-10mee  R225mix  R43-10mee                                    
                                      R225mix                             
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After 6 hours                                                             
         90.0       10.0     90.0     10.0                                
  After 12 hours 90.1 9.9 89.9 10.1                                       
  After 18 hours 90.1 9.9 89.9 10.1                                       
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     EXAMPLE 8 
     The same procedure as in Example 2 was repeated, except that a mixed solvent composition consisting of 50% R43-10mee and 50% of R225mix (R225ca/R225cb=45%/55% mixture) was used as a mixed solvent composition. The results are shown in Table 8. 
     
                       TABLE 8                                                     
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       Composition (%)                                                    
         Cleaning sump   Water separator                                  
Time     R43-10mee  R225mix  R43-10mee                                    
                                      R225mix                             
______________________________________                                    
After 6 hours                                                             
         50.0       50.0     50.0     50.0                                
  After 12 hours 50.0 50.0 50.0 50.0                                      
  After 18 hours 49.9 50.1 50.1 49.9                                      
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     EXAMPLES 9 to 16 
     By using the mixed solvent compositions shown in Table 9, a machine oil cleaning test (A) was carried out. 
     
                       TABLE 9                                                     
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No    Solvent composition                                                 
                      %     Degree of removal A                           
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 9    R43-10mee       55    ⊚                              
   R225ca 45                                                              
  10 R43-10mee 48 ⊚                                        
   R225ca 52                                                              
  11 R43-10mee 40 ⊚                                        
   R225ca 60                                                              
  12 R43-10mee 70 ⊚                                        
   R225cb 30                                                              
  13 R43-10mee 58 ⊚                                        
   R225cb 42                                                              
  14 R43-10mee 50 ⊚                                        
   R225cb 50                                                              
  15 R43-10mee 90 ⊚                                        
   R225ca  4                                                              
   R225cb  6                                                              
  16 R43-10mee 50 ⊚                                        
   R225ca 10                                                              
   R225cb 40                                                              
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     EXAMPLES 17 to 24 
     By using the mixed solvent compositions shown in Tables 10 and 11, a defluxing test (B) was carried out. 
     
                       TABLE 10                                                    
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No    Solvent composition                                                 
                      %     Degree of removal B                           
______________________________________                                    
17    R43-10mee       50    ⊚                              
   R225ca 40                                                              
   2-propanol 10                                                          
  18 R43-10mee 45 ⊚                                        
   R225ca 50                                                              
   methanol  5                                                            
  19 R43-10mee 36 ⊚                                        
   R225ca 56                                                              
   ethanol  8                                                             
  20 R43-10mee 60 ⊚                                        
   R225cb 30                                                              
   methanol 10                                                            
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                       TABLE 11                                                    
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No    Solvent composition                                                 
                      %     Degree of removal B                           
______________________________________                                    
21    R43-10mee       55    ⊚                              
   R225cb 40                                                              
   2-propanol  5                                                          
  22 R43-10mee 47 ⊚                                        
   R225cb 47                                                              
   ethanol  6                                                             
  23 R43-10mee 80 ⊚                                        
   R225ca  4                                                              
   R225cb  6                                                              
   methanol 10                                                            
  24 R43-10mee 50 ⊚                                        
   R225ca 20                                                              
   R225cb 25                                                              
   2-propanol  5                                                          
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     EXAMPLES 25 to 32 
     By using the mixed solvent compositions shown in Tables 12 and 13, a test (C) for removing deposited water was carried out. 
     
                       TABLE 12                                                    
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No    Solvent composition                                                 
                      %     Degree of removal C                           
______________________________________                                    
25    R43-10mee       53    ⊚                              
   R225ca 42                                                              
   2-propanol  5                                                          
  26 R43-10mee 40 ⊚                                        
   R225ca 50                                                              
   ethanol 10                                                             
  27 R43-10mee 35 ⊚                                        
   R225ca 50                                                              
   methanol 15                                                            
  28 R43-10mee 62 ⊚                                        
   R225cb 33                                                              
   methanol  5                                                            
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                       TABLE 13                                                    
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No    Solvent composition                                                 
                      %     Degree of removal C                           
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29    R43-10mee       55    ⊚                              
   R225cb 35                                                              
   ethanol 10                                                             
  30 R43-10mee 46 ⊚                                        
   R225cb 46                                                              
   2-propanol  8                                                          
  31 R43-10mee 85 ⊚                                        
   R225ca  5                                                              
   R225cb  2                                                              
   ethanol  8                                                             
  32 R43-10mee 45 ⊚                                        
   R225ca 10                                                              
   R225cb 35                                                              
   methanol 10                                                            
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     EXAMPLE 33 
     250 cc of a mixed solvent composition of R225ca (b.p. 51.1° C.) and R51-14 (b.p. 56° C.) in such a ratio as shown 14 was charged into an Othmer type gas-liquid equilibrium distillation apparatus, and was heated. After the composition reached equilibrium, samples were taken from the gas phase and the liquid phase and were analyzed by gas chromatography. The results are shown in Table 14. The azeotropic composition was R225ca/R51-14=55.0%/45.0%. 
     
                       TABLE 14                                                    
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Example 33: Gas phase Example 33: Liquid phase                            
  composition (%)  composition (%)                                        
R225ca    R51-14      R225ca    R51-14                                    
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90.0      10.0        94.0       6.0                                      
  75.0 25.0 79.0 21.0                                                     
  55.0 45.0 55.0 45.0                                                     
  43.0 57.0 40.0 60.0                                                     
  30.0 70.0 25.0 75.0                                                     
  14.0 86.0 10.0 90.0                                                     
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     EXAMPLE 34 
     1,000 g of a mixed solvent composition of R225ca/R51-14=30.0%/70.0% was charged into a distillation flask, and the flask was connected to a distillation column having a number of theoretical plates of 5. Then, the composition was heated and fluxed for 2 hours. After the composition reached equilibrium, the fraction was periodically collected and analyzed by gas chromatography. The results are shown in Table 15. 
     EXAMPLE 35 
     The same procedure as in Example 34 was repeated, except that 1,000 g of a mixed solvent composition of R225ca/R51-14=75.0%/25.0% was used as a mixed solvent composition. The results as shown in Table 15. 
     
                       TABLE 15                                                    
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Portion of  Example 34:       Example 35:                                 
  fraction Composition (%)  Composition (%)                               
collected (%)                                                             
            R225ca  R51-14    R225ca                                      
                                    R51-14                                
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20          30.0    70.0      75.0  25.0                                  
  60 30.0 70.0 75.0 25.0                                                  
  80 30.1 69.9 74.9 25.1                                                  
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     EXAMPLE 36 
     The same procedure as in Example 34 was repeated, except that 1,000 g of a mixed solvent composition of R225ca/R51-14/R51-14my/R51-14mcy=30.0%/50.0%/15.0%/5.0% was used as a mixed solvent composition. The results are shown in Table 16. 
     
                       TABLE 16                                                    
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Portion of                                                                
  fraction Example 36:                                                    
  collected Composition (%)                                               
(%)       R225ca  R51-14    R51-14my                                      
                                   R51-14mcy                              
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20        30.0    50.0      15.0   5.0                                    
  60 30.0 50.0 15.0 5.0                                                   
  80 30.1 49.9 15.0 5.0                                                   
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     EXAMPLE 37 
     The same procedure as in Example 34 was repeated, except that 1,000 g of a mixed solvent composition of R225ca/R51-14/R51-14my/R51-14mcy=75.0%/18.0%/5.0%/2.0% as a mixed solvent composition. The results are Table 17. 
     
                       TABLE 17                                                    
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Portion of                                                                
  fraction Example 37:                                                    
  collected Composition (%)                                               
(%)       R225ca  R51-14    R51-14my                                      
                                   R51-14mcy                              
______________________________________                                    
20        75.0    18.0      5.0    2.0                                    
  60 75.0 18.0 5.0 2.0                                                    
  80 74.9 18.1 5.0 2.0                                                    
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     EXAMPLE 38 
     250 cc of a mixed solvent composition of R225cb (b.p. 56.1° C.) and R51-14 (b.p. 56° C.) in such a ratio as shown in Table 18 was charged into an Othmer type gas-liquid equilibrium distillation apparatus, and was heated. After the composition reached equilibrium, samples were taken from the gas phase and the liquid phase and were analyzed by gas chromatography. The results are shown in Table 18. The azeotropic composition was R225cb/R51-14=45.0%/55.0%. 
     
                       TABLE 18                                                    
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Example 38:            Example 38:                                        
  Gas phase  Liquid phase                                                 
  composition (%)  composition (%)                                        
R225cb   R51-14        R225cb  R51-14                                     
______________________________________                                    
20.0     80.0          11.0    89.0                                       
  32.0 68.0 23.0 77.0                                                     
  42.0 58.0 41.0 59.0                                                     
  45.0 55.0 45.0 55.0                                                     
  56.0 44.0 61.0 39.0                                                     
  80.0 20.0 87.0 13.0                                                     
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     EXAMPLE 39 
     The same procedure as in Example 34 was repeated, except that 1,000 g of a mixed solvent composition of R225cb/R51-14=25.0%/75.0% was used as a mixed solvent composition. The results are shown in Table 19. 
     EXAMPLE 40 
     The same procedure as in Example 34 was repeated, except that 1,000 g of a mixed solvent composition of R225cb/R51-14=60.0%/40.0% was used as a mixed solvent composition. The results are shown in Table 19. 
     
                       TABLE 19                                                    
______________________________________                                    
Portion of                                                                
  fraction Example 39:  Example 40:                                       
  collected Composition (%)  Composition (%)                              
(%)        R225cb  R51-14     R225cb                                      
                                    R51-14                                
______________________________________                                    
20         25.0    75.0       60.0  40.0                                  
  60 25.0 75.0 60.0 40.0                                                  
  80 25.1 74.9 59.9 40.1                                                  
______________________________________                                    
 
    
     EXAMPLE 41 
     The same procedure as in Example 34 was repeated, except that 1,000 g of a mixed solvent composition R225cb/R51-14/R51-14my/R51-14mcy=25.0%/47.0%/13.0%/5.0% as a mixed solvent composition. The results are Table 20. 
     
                       TABLE 20                                                    
______________________________________                                    
Portion of                                                                
  fraction Example 41:                                                    
  collected Composition (%)                                               
(%)       R225cb  R51-14    R51-14my                                      
                                   R51-14mcy                              
______________________________________                                    
20        25.0    54.0      16.0   5.0                                    
  60 25.0 54.0 16.0 5.0                                                   
  80 25.1 53.9 16.0 5.0                                                   
______________________________________                                    
 
    
     EXAMPLE 42 
     The same procedure as in Example 34 was repeated, except that 1,000 g of a mixed solvent composition of R225cb/R51-14/R51-14my/R51-14mcy=60.0%/29.0%/8.0%/3.0% as a mixed solvent composition. The results are shown in Table 21. 
     
                       TABLE 21                                                    
______________________________________                                    
Portion of                                                                
  fraction Example 42:                                                    
  collected Composition (%)                                               
(%)       R225cb  R51-14    R51-14my                                      
                                   R51-14mcy                              
______________________________________                                    
20        60.0    29.0      8.0    3.0                                    
  60 60.0 29.0 8.0 3.0                                                    
  80 59.9 29.1 8.0 3.0                                                    
______________________________________                                    
 
    
     EXAMPLE 43 
     The same procedure as in Example 34 was repeated, except that 1,000 g of a mixed solvent composition consisting of 50.0% of R225 of R225ca/R225cb=45/55 (weight ratio) and 50.0% of R51-14 was used as a mixed solvent composition. The results are shown in table 22. 
     EXAMPLE 44 
     The same procedure as in Example 34 was repeated, except that 1000 g of a mixed solvent composition consisting of 25.0% of R225 of R225ca/R225cb=45/55 (weight ratio) and 75.0% of R51-14 was used as a mixed solvent composition. The results are shown in table 22. 
     EXAMPLE 45 
     The same procedure as in Example 34 was repeated, except that 1,000 g of a mixed solvent composition consisting of 70.0% of R225mix of R225ca/R225cb=45/55 (weight ratio) and 30.0% of R51-14 was used as a mixed solvent composition. The results are shown in table 22. 
     
                       TABLE 22                                                    
______________________________________                                    
Portion                                                                   
  of                                                                      
  fraction Example 43: Example 44: Example 45:                            
  collect- Composition (%) Composition (%) Composition (%)                
ed (%)                                                                    
      R225mix  R51-14  R225mix                                            
                              R51-14                                      
                                    R225mix                               
                                           R51-14                         
______________________________________                                    
20    51.0     49.0    25.0   75.0  70.0   30.0                           
  60 51.0 49.0 25.0 75.0 70.0 30.0                                        
  80 51.2 48.8 25.1 74.9 69.9 30.1                                        
______________________________________                                    
 
    
     EXAMPLE 46 
     The same procedure as in Example 34 was repeated, except that 1,000 g of a mixed solvent composition consisting of 25.0% of R225mix of R225ca/R225cb=45/55 (weight ratio), 47.0% of R51-14, 13.0% of R51-14my and 5.0% of R51-14mcy was used as a mixed solvent composition. The results are shown in table 23. 
     
                       TABLE 23                                                    
______________________________________                                    
Portion of                                                                
  fraction Example 46:                                                    
  collected Composition (%)                                               
(%)      R225mix  R51-14    R51-14my                                      
                                   R51-14mcy                              
______________________________________                                    
20       25.0     54.0      16.0   5.0                                    
  60 25.0 54.0 16.0 5.0                                                   
  80 25.1 53.9 16.0 5.0                                                   
______________________________________                                    
 
    
     EXAMPLE 47 
     The same procedure as in Example 34 was repeated, except that 1,000 g of a mixed solvent composition consisting of 55.0% of R225mix of R225ca/R225cb=45/55 (weight ratio), 33.0% of R51-14, 9.0% of R51-14my and 3.0% of R51-14mcy was used as a mixed solvent composition. The results are shown in table 24. 
     
                       TABLE 24                                                    
______________________________________                                    
Portion of                                                                
  fraction Example 47:                                                    
  collected Composition (%)                                               
(%)      R225mix  R51-14    R51-14my                                      
                                   R51-14mcy                              
______________________________________                                    
20       55.0     33.0      9.0    3.0                                    
  60 55.0 33.0 9.0 3.0                                                    
  80 55.1 32.9 9.0 3.0                                                    
______________________________________                                    
 
    
     EXAMPLE 48 
     The same procedure as in Example 34 was repeated, except that 1,000 g of a mixed solvent composition consisting of 45.0% of R225mix of R225ca/R225cb=45/55 (weight ratio), 40.0% of R51-14, 11.0% of R51-14my and 4.0 of R51-14mcy was used as a mixed solvent ion. The results are shown in table 25. 
     
                       TABLE 25                                                    
______________________________________                                    
Portion of                                                                
  fraction Example 48:                                                    
  collected Composition (%)                                               
(%)      R225mix  R51-14    R51-14my                                      
                                   R51-14mcy                              
______________________________________                                    
20       45.0     40.0      11.0   4.0                                    
  60 45.0 40.0 11.0 4.0                                                   
  80 44.9 40.1 11.0 4.0                                                   
______________________________________                                    
 
    
     EXAMPLE 49 
     The same procedure as in Example 34 was repeated, except that 1,000 g of a mixed solvent composition consisting of 70.0% of R225mix of R225ca/R225cb=45/55 (weight ratio), 22.0% of R51-14, 6.0% of R51-14my and 2.0 of R51-14mcy was used as a mixed solvent on. The results are shown in table 26. 
     
                       TABLE 26                                                    
______________________________________                                    
Portion of                                                                
  fraction Example 49:                                                    
  collected Composition (%)                                               
(%)      R225mix  R51-14    R51-14my                                      
                                   R51-14mcy                              
______________________________________                                    
20       70.0     22.0      6.0    2.0                                    
  60 70.0 22.0 6.0 2.0                                                    
  80 69.9 22.1 6.0 2.0                                                    
______________________________________                                    
 
    
     EXAMPLES 50 to 60 
     By using the mixed solvent compositions shown in Table 27, a machine oil cleaning test (A) was carried out. 
     
                                           TABLE 27                                
__________________________________________________________________________
     Solvent  Degree of  Solvent  Degree of                               
  Example Composition % removal A Example Composition % removal A         
__________________________________________________________________________
50   R225ca                                                               
           30 ⊚                                            
                   56    R225cb                                           
                               45 ⊚                        
   R51-14 50   R51-14 55                                                  
   R51-14my 15  57 R225cb 60 ⊚                             
   R51-14mcy 5   R51-14 29                                                
  51 R225ca 40 ⊚  R51-14my 8                               
   R51-14 60   R51-14mcy 3                                                
  52 R225ca 55 ⊚ 58 R225ca 10 ⊚             
   R51-14 45   R225cb 15                                                  
  53 R225ca 75 ⊚  R51-14 54                                
   R51-14 18   R51-14my 16                                                
   R51-14my 5   R51-14mcy 5                                               
   R51-14mcy 2  59 R225ca 25 ⊚                             
  54 R225cb 25 ⊚  R225cb 25                                
   R51-14 54   R51-14 50                                                  
   R51-14my 16  60 R225ca 40 ⊚                             
   R51-14mcy 5   R225cb 30                                                
  55 R225cb 50 ⊚  R51-14 22                                
   R51-14 50   R51-14my 6                                                 
       R51-14mcy 2                                                        
__________________________________________________________________________
 
    
     EXAMPLES 61 to 69 
     By using the mixed solvent compositions shown in Table 28 and 29, defluxing test (B) and a test (C) for removing deposited water were carried out. 
     
                       TABLE 28                                                    
______________________________________                                    
          Solvent            Degree of                                    
                                    Degree of                             
  Example Composition % removal B removal C                               
______________________________________                                    
61        R225ca    25       ⊚                             
                                    ⊚                      
   R51-14 47                                                              
   R51-14my 13                                                            
   R51-14mcy 5                                                            
   methanol 10                                                            
  62 R225ca 40 ⊚ ⊚                          
   R51-14 50                                                              
   ethanol 10                                                             
  63 R225ca 68 ⊚ ⊚                          
   R51-14 20                                                              
   R51-14my 5                                                             
   R51-14mcy 2                                                            
   2-propanol 5                                                           
  64 R225cb 25 ⊚ ⊚                          
   R51-14 47                                                              
   R51-14my 13                                                            
   R51-14mcy 5                                                            
   ethanol 10                                                             
  65 R225cb 40 ⊚ ⊚                          
   R51-14 55                                                              
   2-propanol 5                                                           
______________________________________                                    
 
    
     
                       TABLE 29                                                    
______________________________________                                    
          Solvent            Degree of                                    
                                    Degree of                             
  Example Composition % removal B removal C                               
______________________________________                                    
66        R225cb    50       ⊚                             
                                    ⊚                      
   R51-14 25                                                              
   R51-14my 7                                                             
   R51-14mcy 3                                                            
   methanol 15                                                            
  67 R225ca 10 ⊚ ⊚                          
   R225cb 45                                                              
   R51-14 29                                                              
   R51-14my 8                                                             
   R51-14mcy 3                                                            
   2-propanol 5                                                           
  68 R225ca 20 ⊚ ⊚                          
   R225cb 20                                                              
   R51-14 50                                                              
   methanol 10                                                            
  69 R225ca 5 ⊚ ⊚                           
   R225cb 25                                                              
   R51-14 40                                                              
   R51-14my 11                                                            
   R51-14mcy 4                                                            
   ethanol 15                                                             
______________________________________                                    
 
    
     EXAMPLE 70 
     1,000 g of a mixed solvent composition consisting of 45% of R225mix (R225ca/R225cb =45%/55%), 45% of R51-14 and 10% of methanol (MeOH) was charged into a of 5 distillation flask, and the flask was connected to a distillation column having a number of theoretical plates of 5. Then, the composition was heated and refluxed for 2 hours. After the composition reached equilibrium, the fraction was periodically collected and analyzed by gas chromatography. The results are shown in Table 30. 
     EXAMPLE 71 
     The same procedure as in Example 70 was repeated, except that 1,000 g of a mixed solvent composition consisting of 35% of R225mix (R225ca/R225cb=45%/55%), 62% of R51-14 and 3% of MeOH was used as a mixed solvent composition. The results are shown in Table 30. 
     
                       TABLE 30                                                    
______________________________________                                    
Portion of                                                                
  fraction Example 70: Example 71:                                        
  collected Composition (%) Composition (%)                               
(%)    R225mix  R51-14  MeOH  R225mix                                     
                                     R51-14                               
                                           MeOH                           
______________________________________                                    
20     45.0     45.0    10.0  35.0   62.0  3.0                            
  40 45.0 45.0 10.0 35.0 62.0 3.0                                         
  60 45.1 44.9 10.0 34.9 62.1 3.0                                         
______________________________________                                    
 
    
     EXAMPLE 72 
     The same procedure as in Example 70 was repeated, except that 1,000 g of a mixed solvent composition consisting of 40% of R225mix (R225ca/R225cb=45%/55%), 36% of R51-14, 10% of R51-14my, 4% of R51-14mcy and 10% of MeOH was used as a mixed solvent composition. The results are shown in Table 31. 
     
                       TABLE 31                                                    
______________________________________                                    
Portion of                                                                
  fraction Example 72:                                                    
  collected Composition (%)                                               
(%)    R225mix  R51-14   R51-14my                                         
                                R51-14mcy                                 
                                         MeOH                             
______________________________________                                    
20     40.0     36.0     10.0   4.0      10.0                             
  40 40.0 36.0 10.0 4.0 10.0                                              
  60 39.9 36.1 10.0 4.0 10.0                                              
______________________________________                                    
 
    
     EXAMPLE 73 
     The same procedure as in Example 70 was repeated, except that 1,000 g of a mixed solvent composition consisting of 50% of R225mix (R225ca/R225cb=45%/55%), 34% of R51-14, 9% of R51-14my, 4% of R51-14mcy and 3% of MeOH was used as a mixed solvent composition. The results are shown in Table 32. 
     
                       TABLE 32                                                    
______________________________________                                    
Portion of                                                                
  fraction Example 73: Composition (%)                                    
collected (%)                                                             
        R225mix  R51-14   R51-14my                                        
                                 R51-14mcy                                
                                         MeOH                             
______________________________________                                    
20      50.0     34.0     9.0    4.0     3.0                              
  40 50.0 34.0 9.0 4.0 3.0                                                
  60 50.1 33.9 9.0 4.0 3.0                                                
______________________________________                                    
 
    
     EXAMPLE 74 
     The same procedure as in Example 70 was repeated, except that 1,000 g of a mixed solvent composition consisting of of 20% of R225mix (R225ca/R225cb=45%/55%), 75% of R51-14 and 5% of MeOH was used as a mixed solvent composition. The results are shown in Table 33. 
     
                       TABLE 33                                                    
______________________________________                                    
Portion of fraction                                                       
             Example 74: Composition (%)                                  
collected (%)                                                             
             R225mix     R51-14  MeOH                                     
______________________________________                                    
20           20.0        75.0    5.0                                      
  40 20.0 75.0 5.0                                                        
  60 19.9 75.1 5.0                                                        
______________________________________                                    
 
    
     EXAMPLE 75 
     The same procedure as in Example 70 was repeated, that 1,000 g of a mixed solvent composition consisting of 45% of R225mix (R225ca/R225cb=45%/55%), 47% of R51-14 and 8% of ethanol (EtOH) was used as a mixed solvent composition. The results are shown in Table 34. 
     EXAMPLE 76 
     The same procedure as in Example 70 was repeated, that 1,000 g of a mixed solvent composition consisting of 28% of R225mix (R225ca/R225cb=45%/55%), 69% of R51-14 and 3% of EtOH was used as a mixed solvent composition. The results are shown in Table 34. 
     
                       TABLE 34                                                    
______________________________________                                    
Portion of                                                                
  fraction Example 75: Example 76:                                        
  collected Composition (%) Composition (%)                               
(%)    R225mix  R51-14  EtOH  R225mix                                     
                                     R51-14                               
                                           EtOH                           
______________________________________                                    
20     45.0     47.0    8.0   28.0   69.0  3.0                            
  40 45.0 47.0 8.0 28.0 69.0 3.0                                          
  60 45.1 46.9 8.0 27.9 69.1 3.0                                          
______________________________________                                    
 
    
     The same procedures as in Example 70 was repeated, exept that 1000 
     EXAMPLE 77 
     The same procedure as in Example 70 was repeated, except that 1,000 g of a mixed solvent composition consisting of 30% of R225mix (R225ca/R225cb=45%/55%), 45% of R51-14, 12% of R51-14my, 5% of R51-14mcy and 8% of EtOH was used as a mixed solvent composition. The results are shown in Table 35. 
     
                       TABLE 35                                                    
______________________________________                                    
Portion of                                                                
  fraction Example 77: Composition (%)                                    
collected (%)                                                             
        R225mix  R51-14   R51-14my                                        
                                 R51-14mcy                                
                                         EtOH                             
______________________________________                                    
20      30.0     45.0     12.0   5.0     8.0                              
  40 30.0 45.0 12.0 5.0 8.0                                               
  60 29.9 45.1 12.0 5.0 8.0                                               
______________________________________                                    
 
    
     EXAMPLE 78 
     The same procedure as in Example 70 was repeated, except that 1,000 g of a mixed solvent composition consisting of 28% of R225mix (R225ca/R225cb=45%/55%), 50% of R51-14, 13% of R51-14my, 6% of R51-14mcy and 3% of EtOH was used as a mixed solvent composition. The results are shown in Table 36. 
     
                       TABLE 36                                                    
______________________________________                                    
Portion of                                                                
  fraction Example 78: Composition (%)                                    
collected (%)                                                             
        R225mix  R51-14   R51-14my                                        
                                 R51-14mcy                                
                                         EtOH                             
______________________________________                                    
20      28.0     50.0     13.0   6.0     3.0                              
  40 28.0 50.0 13.0 6.0 3.0                                               
  60 27.9 50.1 13.0 6.0 3.0                                               
______________________________________                                    
 
    
     EXAMPLE 79 
     The same procedure as in Example 70 was repeated, except that 1,000 g of a mixed solvent composition consisting of 20% of R225mix (R225ca/R225cb=45%/55%), 75% of 51-14 and 5% of EtOH was used as a mixed solvent composition. The results are shown in Table 37. 
     
                       TABLE 37                                                    
______________________________________                                    
Portion of fraction                                                       
             Example 79: Composition (%)                                  
collected (%)                                                             
             R225mix      R51-14  EtOH                                    
______________________________________                                    
20           20.0         75.0    5.0                                     
  40 20.0 75.0 5.0                                                        
  60 19.9 75.1 5.0                                                        
______________________________________                                    
 
    
     EXAMPLE 80 
     The same procedure as in Example 70 was repeated, except that 1,000 g of a mixed solvent composition consisting of 20% of R225mix (R225ca/R225cb=45%/55%), 73% of R51-14 and 7% of 2-propanol (2-PrOH) was used as a mixed solvent composition. The results are shown in Table 38. 
     EXAMPLE 81 
     The same procedure as in Example 70 was repeated, except that 1,000 g of a mixed solvent composition consisting of 60% of R225mix (R225ca/R225cb=45%/55%), 38.5% of R51-14 and 1.5% of 2-PrOH was used as a mixed solvent composition. The results are shown in Table 38. 
     
                       TABLE 38                                                    
______________________________________                                    
Portion of                                                                
  fraction Example 80: Example 81:                                        
  collected Composition (%) Composition (%)                               
(%)    R225mix  R51-14  2-PrOH                                            
                              R225mix                                     
                                     R51-14                               
                                           2-PrOH                         
______________________________________                                    
20     20.0     73.0    7.0   60.0   38.5  1.5                            
  40 20.0 73.0 7.0 60.0 38.5 1.5                                          
  60 20.1 72.9 7.0 59.9 38.6 1.5                                          
______________________________________                                    
 
    
     EXAMPLE 82 
     The same procedure as in Example 70 was repeated, except that 1,000 g of a mixed solvent composition consisting of 30% of R225mix (R225ca/R225cb=45%/55%), 46% of R51-14, 12% of R51-14my, 5% of R51-14mcy and 7% of 2-PrOH was used as a mixed solvent composition. The results are shown in Table 39. 
     
                       TABLE 39                                                    
______________________________________                                    
Portion of                                                                
  fraction Example 82: Composition (%)                                    
collected (%)                                                             
        R225mix  R51-14   R51-14my                                        
                                 R51-14mcy                                
                                         2-PrOH                           
______________________________________                                    
20      30.0     46.0     12.0   5.0     7.0                              
  40 30.0 46.0 12.0 5.0 7.0                                               
  60 29.9 46.1 12.0 5.0 7.0                                               
______________________________________                                    
 
    
     EXAMPLE 83 
     The same procedure as in Example 70 was repeated, except that 1,000 g of a mixed solvent composition consisting of 50% of R225mix (R225ca/R225cb=45%/55%), 35% of R51-14, 9% of R51-14my, 4.5% of R51-14mcy and 1.5% of 2-PrOH was used as a mixed solvent composition. The are shown in Table 40. 
     
                       TABLE 40                                                    
______________________________________                                    
Portion of                                                                
  fraction Example 83: Composition (%)                                    
collected (%)                                                             
        R225mix  R51-14   R51-14my                                        
                                 R51-14mcy                                
                                         2-PrOH                           
______________________________________                                    
20      50.0     35.0     9.0    4.5     1.5                              
  40 50.0 35.0 9.0 4.5 1.5                                                
  60 50.1 34.9 9.0 4.5 1.5                                                
______________________________________                                    
 
    
     EXAMPLE 84 
     The same procedure as in Example 70 was repeated, except that 1,000 g of a mixed solvent composition consisting of 20% of R225mix (R225ca/R225cb=45%/55%), 75% of R51-14 and 5% of 2-PrOH was used as a mixed composition. The results are shown in Table 41. 
     
                       TABLE 41                                                    
______________________________________                                    
Portion of fraction                                                       
             Example 84: Composition (%)                                  
collected (%)                                                             
             R225mix      R51-14  2-PrOH                                  
______________________________________                                    
20           20.0         75.0    5.0                                     
  40 20.0 75.0 5.0                                                        
  60 20.1 74.9 5.0                                                        
______________________________________                                    
 
    
     EXAMPLES 85 to 98 
     By using the mixed solvent compositions shown in Table 42 (R225mix is a mixture of R225ca/R225cb=45%/55%), a machine oil cleaning test (A), a defluxing test (B) and a test (C) for removing deposited water were carried out. In Table 42, A, B and C indicate the degrees of removal A, B and C of the respective tests. 
     
                       TABLE 42                                                    
______________________________________                                    
Example                                                                   
       Solvent composition                                                
                        %         A   B    C                              
______________________________________                                    
85     R225mix/R51-14/MeOH                                                
                        45/45/10  ⊚                        
                                      ⊚                    
                                           ⊚               
  86 R225mix/R51-14/MeOH 35/62/3 ⊚ ⊚        
                                           ⊚               
  87 R225mix/R51-14/R51-14my/ 40/36/10/4/ ⊚ .circleincircle
                                           . ⊚             
   R51-14mcy/MeOH 10                                                      
  88 R225mix/R51-14/R51-14my/ 50/34/9/ ⊚ ⊚  
                                           ⊚               
   R51-14mcy/MeOH 4/3                                                     
  89 R225mix/R51-14/EtOH 45/47/8 ⊚ ⊚        
                                           ⊚               
  90 R225mix/R51-14/EtOH 28/69/3 ⊚ ⊚        
                                           ⊚               
  91 R225mix/R51-14/R51-14my/ 30/45/12/5/ ⊚ .circleincircle
                                           . ⊚             
   R51-14mcy/EtOH 8                                                       
  92 R225mix/R51-14/R51-14my/ 28/50/13/6/ ⊚ .circleincircle
                                           . ⊚             
   R51-14mcy/EtOH 3                                                       
  93 R225mix/R51-14/R51-14my/ 30/45/12/5/ ⊚ .circleincircle
                                           . ⊚             
   R51-14mcy/EtOH/2-PrOH 6/2                                              
  94 R225mix/R51-14/R51-14my/ 30/45/12/5/ ⊚ .circleincircle
                                           . ⊚             
   R51-14mcy/EtOH/MeOH 6/2                                                
  95 R225mix/R51-14/2-PrOH 20/73/7 ⊚ ⊚      
                                           ⊚               
  96 R225mix/R51-14/2-PrOH 66/38.5/1.5 ⊚ ⊚  
                                           ⊚               
  97 R225mix/R51-14/R51-14my/ 30/46/12/5/ ⊚ .circleincircle
                                           . ⊚             
   R51-14mcy/2-PrOH 7                                                     
  98 R225mix/R51-14/R51-14my/ 50/35/9/ ⊚ ⊚  
                                           ⊚               
   R51-14mcy/2-PrOH 4.5/1.5                                               
______________________________________