United States Environmental Protection Agency National Kisk Management Research Laboratory Cincinnati, OH 45268 Research and Development EPA/600/SR-95/113 February 1996 & EPA Project Summary New Chemical Alternatives for the Protection of Stratospheric Ozone Darryl D. DesMarteau and Adolph L. Beyerlein Chlorofluorocarbons (CFCs) and their brominated analogs (halons) are rec- ognized as potent contributors to deple- tion of the Earth's stratospheric ozone layer. By international agreement, such chemicals are to be phased out of the worldwide market. Additionally, certain partially halogenated CFCs (or hydrochlorofluorocarbons, HCFCs) have likewise been recognized as stratospheric ozone depleters and are also to be phased out of production by developed countries in a step-wise progression over the period 1996 to 2030. Because of the enormous commer- cial importance of the CFCs, HCFCs, and halons, and because few chemi- cals were readily available or had been proven acceptable for use in the nu- merous applications in which the ozone-depleting substances were em- ployed, the U. S. Environmental Pro- tection Agency and the Electric Power Research Institute sponsored a study of additional potential alternative chemi- cals. This study focused on the investiga- tion of fluorinated derivatives of pro- pane and butane to determine if syn- thesis routes of such compounds were feasible and economical, and to mea- sure the physical properties needed to evaluate the compounds as alterna- tives. This work resulted in the investi- gation of 25 compounds including 15 hydrofluorocarbons (MFCs), 9 HCFCs, and 1 hydrofluoroether (HFE). Several of the compounds studied had not been previously synthesized and, for many of those which had been reported in the literature, this study resulted in im- proved synthesis methods. Also, most compounds which had a prior litera- ture reference had only a boiling point measurement. This study, in addition to the synthesis effort, resulted in a sizeable body of thermophysical prop- erty data for each chemical. This Project Summary was developed by the National Risk Management Re- search Laboratory's Air Pollution Pre- vention and Control Division, Research Triangle Park, NC, to announce key findings of the research project that is fully documented in a separate report of the same title (see Project Report ordering information at back). Introduction Twenty-four fluorinated propane and bu- tane derivatives and one fluorinated ether were evaluated as possible alternatives for CFCs and long-lived HCFCs. Boiling points for these chemicals range from -34.6 to 76.7°C. Therefore, these chemicals pro- vide potential alternatives for a broad range of applications, e.g., as refriger- ants, foam blowing agents, and solvents. Emphasis is on hydrogen-containing com- pounds that are expected to have finite atmospheric lifetimes which reduce their global warming potential. Sixteen of the chemicals investigated contain no chlo- rine or bromine and therefore have zero ozone depletion potential. The remaining nine chlorine-containing chemicals were selected for investigation before regula- tory restrictions were imposed on HCFCs. Nevertheless, the low chlorine content of ------- the nine HCFCs studied, coupled with a finite atmospheric lifetime, may in some cases yield an alternative with a negligible ozone depletion potential. Selection and evaluation of the com- pounds as alternatives require: (1) a knowl- edge of appropriate physical properties and (2) possible synthesis routes. Both of these requirements were investigated in this research. This study emphasized syn- thesis routes using relatively inexpensive commercially available starting materials and established synthesis procedures (chlorination, hydrogenation, and addition of hydrogen fluoride) which are carried out industrially. This is important in order for a chemical to be an economically vi- able alternative for other than a small spe- cialty market. Experimental Procedure Except for one hydrofluoroether (HFE- 125), which was obtained commercially with 98% purity and then repurified, all samples employed for property measure- ments were synthesized with at least 99.5% purity. Synthesized chemicals were identified and their purity checked by a combination of nuclear magnetic reso- nance spectrometry, high pressure Fou- rier transform infrared spectrometry, gas chromatography, and mass spectrometry. Melting point, boiling point, vapor pres- sures below the boiling point, critical tem- perature, critical density, liquid densities, and heat of vaporization at the boiling point were measured for all 25 compounds. For four compounds (HFE-125, HFC- 227ea, HFC236ea, and HFC-245cb), the vapor pressure was measured as a func- tion of temperature to within 1% accuracy from below the boiling point to the critical temperature. Vapor density in the liquid-vapor coex- istence region and vapor pressure between the boiling point and the critical point were estimated by a modified corresponding states technique. The reference fluid for the modified corresponding states calcu- lations was commercially available HFC- 134a (1,1,1,2-tetrafluoroethane), and the equation of state used for the reference fluid was the modified Benedict-Webb- Rubin equation. Heats of vaporization be- tween the boiling point and critical point were calculated from the heat of vaporiza- tion at the boiling point, the boiling point temperature, and the critical temperature. Ideal gas heat capacities and vapor-phase thermal conductivities were estimated by functional group additivity methods. Results Table 1 lists the 25 compounds investi- gated by ASHRAE (American Society of Heating, Refrigerating and Air-Condition- ing Engineers) refrigerant code designa- tion and by chemical formula. Table 1. Compounds Investigated by ASHRAE Refrigerant Designation and Chemical Formula Compound (ASHRAE Code) HFE-125 HFC-227ea HFC-227ca HFC-236fa HFC-236ea HFC-236cb HFC-236ca HFC-245fa HFC-245ca HFC-245cb HFC-254cb HFC-329ccb HFC-338eea HFC-338cca HFC-338ccb HFC-347ccd HCFC-225ba HCFC-225da HCFC-226da HCFC-226ea HCFC-234da HCFC-235ca HCFC-243da HCFC-244ca cy-HCFC-326d Chemical Formula CF3OCF2H CF3CHFCF3 CF3CF2CF2H CF3CH2CF3 CF3CHFCF2H CF3CF2CFH2 CF/YCF2CF2H CF3CH2CF2H CHF2CF2CFH2 CF3CF2CH3 CF2HCF2CH3 CF3CF2CF2CF/Y CF3CFHCFHCF3 CHF2CF2CF2CF/Y CF3CF2CF2CFH2 CF3CF2CF2CH3 CF3CFCICFHCI CF3CHCICF2CI CF3CHCICF3 CF3CHFCF2CI CF3CHCICFHCI CF3CF2CH2CI CF3CHCICH2CI CF//CF2CH2C/ cy-(CFJ3CHCI Table 2 lists the 25 compounds studied along with their boiling point (Tb), melting point (TJ, heat of vaporization at the boil- ing point (AH ), critical temperature (Tc), critical pressure (Pc), critical density (dc), and liquid heat capacity at 40°C (Cpl). Conclusions From the data acquired in this study, it appears that several of the chemicals syn- thesized are worthy of consideration as alternatives to the ozone-depleting CFCs and HCFCs. Table 3 presents selected apparent best candidate alternatives from this study based on a comparison of their thermophysical properties with those of commercially important CFCs and HCFCs and the fact that these candidates have zero ozone depletion potentials. Also, pref- erence was given to fluorinated propanes over fluorinated butanes on the premise that the latter would likely be more expen- sive to produce (cost generally correlates with total fluorine content) and that, for insulation foam production, the butane de- rivatives would likely have higher vapor thermal conductivities than the propane derivatives. These presumptions are some- what tenuous, however, and the possibil- ity that certain of the fluorinated butanes may be excellent candidates should not be discounted. No fluorinated propane derivatives with as low a boiling point as that of CFC-12 (dichlorodifluoromethane, Tb = -29.8°C) were found. After some searching, HFC- 245cb was synthesized with a boiling point of -18.3°C. Its critical temperature of 108.5°C compares well with the critical temperature of CFC-12 (112°C). There- fore, HFC-245cb might be an alternative for CFC-12 for some applications as would HFC-227ca and -227ea with boiling points of-16.3 and -18.3°C, and critical tempera- tures of 106.3 and 102.8°C, respectively. HFE-125, with a boiling point of -34.6°C and critical temperature of 80.7°C, appears to be the best candidate alternative for CFC-115( 1,1,1,2,2-pentafluorochloroethane, Tb = -39.2°C, Tc = 79.9°C) and HCFC-22 (difluorochloromethane, Tb = -40.6°C, T = 96.15°C). HFC-245ca and -245fa with boiling points of 25.0 and 15.3°C and critical temperatures of 178.4 and 157.5°C, re- spectively, are promising candidates to replace CFC-11 (fluorotrichloromethane, T = 23.8°C, T = 198.1°C), HCFC-123 (1,1,1-trifluoro-2,2-dichloroethane, T = 27.9°C, Tc = 183.8°C), and HCFC-141b (1-fluoro-1,1-dichloroethane, Tb = 32.2°C, Tc = 204.2°C) as a refrigerant in low pres- sure chillers and/or as a blowing agent in the manufacture of polyisocyanurate in- sulation foam. All HFC-245 isomers pos- sess a hydrogen content sufficient to pos- sibly render them borderline flammable. Therefore, the flammabilities of these chemicals should be evaluated. A number of CFC-114 (1,1,2,2,- tetrafluoro-1,2,-dichloroethane, Tb = 3.7°C, Tc = 145.7°C) alternatives are possible from the chemicals synthesized. HFCs- 236ea, -236fa, and -236cb with boiling points of 6.5, -1.1, and -1.4°C, respec- tively, and HFC-254cb with a boiling point of -0.8°C are especially attractive. How- ever, the relatively high hydrogen-to-fluo- rine atom ratio of HFC-254cb poses a flammability concern for this compound. ------- Table 2. Boiling Point, Melting Point, Critical Properties, Heat of Vaporization at the Boiling Point, and Liquid-Phase Heat Capacity for the 25 Compounds Studied. Compound HFE-125 HFC-227ea HFC-227ca HFC-236fa HFC-236ea HFC-236cb HFC-236ca HFC-245fa HFC-245ca HFC-245cb HFC-254cb HFC-329ccb HFC-338eea HFC-338cca HFC-338ccb HFC-347ccd HCFC-226da HCFC-226ea HCFC-235ca HCFC-244ca HCFC-225da HCFC-225ba HCFC-234da HCFC-243da cy-HCFC-326d Tb(°C) -34.6 -18.3 -16.3 -1.1 6.5 -1.4 12.6 15.3 25.0 -18.3 -0.8 15.1 25.4 42.5 27.8 15.1 14.1 17.6 28.1 54.8 50.8 51.9 70.1 76.7 38.1 Tm(°C) -156.1 -126.8 -140.3 -94.2 -146.1 -105.4 -123.3 -102.1 -73.4 -81.1 -121.1 -122.3 -91.5 -91.0 -119.4 -124.9 -119.6 -134.0 -85.0 -101.8 -130.3 -132.7 -98.0 -71.6 -94.8 (kJ/mof) 21.92 22.29 23.69 25.66 26.83 25.25 26.59 27.96 29.21 23.59 24.86 26.71 27.79 31.13 26.36 25.82 24.64 26.26 27.57 31.07 25.89 29.38 31.70 30.86 28.69 TC(°C) 80.7 102.8 106.3 130.6 141.1 130.1 155.2 157.5 178.4 108.5 146.1 140.2 148.5 186.4 160.5 144.2 158.2 158.3 170.3 221.0 206.2 212.9 242.5 251.9 196.9 Pc (kPa) 3253 2943 2874 3177 3533 3118 3405 3623 3855 3264 3753 2391 2475 2792 2552 2570 3024 2939 3084 3714 3006 3074 3353 3496 2749 dc (kg/m3) 584 580 594 556 571 545 558 529 529 499 467 600 581 578 562 532 591 584 550 525 589 586 552 514 515 cpl (kJ/kg °C) 1.327 1.258 1.254 1.371 1.304 1.438 NA 1.422 1.454 1.457 1.590 1.223 NA 1.333 1.342 1.383 1.207 1.205 1.275 1.160 1.087 1.087 1.176 1.234 1.158 NA = not available Table 3. Selected Possible Alternatives for Commercially Important CFCs and HCFCs CFCorHCFC To Be Replaced ASHRAE Code of Alternative Chemical Formula of Alternative Chemical Name of Alternative CFC-11, HCFC-123, HCFC-141b CFC-12 CFC-114 CFC-115, HCFC-22 HFC-245ca HFC-245fa HFC-227ea HFC-227ca HFC-245cb HFC-236ea HFC-236fa HFC-236cb HFC-254cb HFE-125 CF/YCF2CFH2 CF3CH2CF2H CF3CHFCF3 CF3CF2CF/y CF3CF2CH3 CF3CHFCF2H CF3CH2CF3 CF3CF2CFH2 CF/YCF2CH3 CFjOCF/Y 1,1,2,2,3-pentafluoropropane 1,1,1,3,3-pentafluoropropane 1,1,1,2,3,3,3-heptafluoropropane 1,1,1,2,2,3,3-heptafluoropropane 1,1,1,2,2-pentafluoropropane 1,1,1,2,3,3-hexafluoropropane 1,1,1,2,2,2-hexafluoropropane 1,1,1,2,2,3-hexafluoropropane 1,1,2,2-tetrafluoropropane pentafluorodimethylether ------- D. DesMarteau and A. Beyerlein are with Clemson University, Clemson, SC 29634. N. Dean Smith is the EPA Project Officer (see below). The complete report, entitled "New Chemical Alternatives for the Protectin of Stratospheric Ozone," (Order No. PB95-260220; Cost $27.00, subject to change) will be available only from: National Technical Information Service 5285 Port Royal Road Springfield, VA 22161 Telephone: 703-487-4650 The EPA Project Officer can be contacted at: Air Pollution Prevention and Control Division National Risk Management Research Laboratory U.S. Environmental Protection Agency Research Triangle Park, NC 27711 United States Environmental Protection Agency National Risk Management Research Laboratory (G-72) Cincinnati, OH 45268 Official Business Penalty for Private Use $300 BULK RATE POSTAGE & FEES PAID EPA PERMIT No. G-35 EPA/600/SR-95/113 ------- |