FLASH POINT DETERMINATION OF BINARY MIXTURES OF ALCOHOLS, KETONES AND WATER. P.J. Martínez, E. Rus and J.M. Compaña

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1 FLASH POINT DETERMINATION OF BINARY MIXTURES OF ALCOHOLS, KETONES AND WATER Abstract P.J. Martínez, E. Rus and J.M. Compaña Departamento de Ingenería Químca. Facultad de Cencas. Unversdad de Málaga Málaga (SPAIN) The flash pont of pure organc compounds, ther mxtures, and ther mxtures wth water s a datum of great nterest toward the preventon of accdents when usng chemcals as a consequence of fres and explosons that may be orgnated by the substance/mxture when get n contact wth the oxygen n the presence of an gnton source, just as the fre trangle establshes. The flash pont of a substance or mxture of substances s a varable of necessary knowledge to determne the fre and exploson rsks, provdng an ndex for hs classfcaton (.e., Code of Federal Regulatons of the Department of Transport, or the NFPA 30, both of U.S.A.). In ths researchng work, some alcohols and ketones of common use as solvents or smlar were choosed. Then, the flash pont of dverse mxtures alcohol-alcohol, alcohol-water, alcohol-ketone, ketoneketone, and ketone-water were determned expermentally. Later on, the obtaned expermental data were analyzed, to estmate the flash pont theoretcally wth approprate accuracy usng dverse models and correlatons to obtan the dverse necessary parameters. So for the vapor pressure of the pure compounds (P sat ), the followng equatons were used: Antone, Clausus-Clapeyron, and so on. To determne the actvty coeffcents of the dfferent components n the lqud mxture (γ ) equatons lke Margules, Van Laar, and UNIFAC were used. For the determnaton of the lower flammablty lmt (LFL ) the equatons of Hanley, Prugh, Le Chateler, and Kanury were used. Lastly, the dfferent proposed procedures to estmate the flash pont were compared, determnng those that offer better results, when contrastng wth the obtaned expermental results. 1. INTRODUCTION The flash pont of a chemcal or a mxture of several chemcals s a varable of man nterest when we evaluate the safety of a product or a process (Law and Chu (2003)). The data of pure compounds are usually avalable, but there s only a lttle nformaton about the emprcal behavour of mxtures. In a prevous work (Martínez et al. (2002)), a frst attempt n ths way for some bnary mxtures alcohol-water was publshed. Some authors have studed several aspects of ths problem.e. Suzuk et al. (1990), Gmehlng and Rasmussen (1982), Hanley (1998) and Lenor (1975), but there s not very much nformaton about a general method or equaton to determne flash pont based on expermental data. 2. CHEMICALS AND EQUIPMENT 2.1. Chemcals In ths work, we have selected some common ndustral alcohols and ketones wdely used n the ndustry as solvents or reagents towards obtan mxtures of practcal mportance. The man crteron to select the chemcals has been the mportance gven to them n Papa and Sherman (1981), Parrsh (1983), Falbe et al. (2003), Segel and 1

2 Eggersdorfer (2003), Stoye (2003) and Werle and Morawetz (2003). Specfcally, the solvents selected, wth ther physcal propertes, the presented n table 1: TABLE 1: The studed compounds and ther physcal propertes. COMPOUND MW BP D 20 ºC FP LFL H v (g/mol) (ºC) (g/cm 3 ) (ºC) (%) (kj/mol) Acetone Acetophenone Dacetone alcohol Dsobutyl ketone Ethanol Ethylene glycol Isobutanol Methanol Methyl ethyl ketone Methyl sobutyl ketone propanol propanol Water N.F. N.F Wth these chemcals, we prepared samples of bnary mxtures wth a known composton Equpment An Automatc Flash Pont Tester Abel IP 170 Herzog MC 306, coupled to a cooler model LAUDA RK 8 CS was used. Ths equpment s adequate to measure flash ponts between 40 and 0 ºC wth an ethylene glycol-water coolng mxture. In addton, a Flash Pont analyzer Herzog HFP Pensky Martens was used. Wth ths one, flash ponts between and 370 ºC can be measured. 3. EXPERIMENTAL Once the composton of the desred sample s selected, t s prepared n a volume of 78.5 ml as t s establshed n the IP 170 standard. The selected sample s then ntroduced n the sample vessel of the apparatus. The expected flash pont s programmed n the frontal board, and the test s run. The results of all tests are repeated twce more, and the mean s calculated. The expermental data measured for some representatve bnary mxtures selected between the prepared, are resumed n the followng tables, 2 to 11, where x s the molar fracton, and FP s the flash pont: Table 2: Flash pont of mxtures acetone-water x FP(ºC) Table 3: Flash pont of mxtures methanol-water x FP (ºC)

3 Table 4: Flash pont of mxtures ethanol-water x FP (ºC) Table 5: Flash pont of mxtures 1-propanol-water x FP (ºC) Table 6: Flash pont of mxtures 2-propanol-water x FP (ºC) Table 7: Flash pont of mxtures sobutanol-water x FP (ºC) Table 8: Flash pont of mxtures 1-propanol-ethylene glycol x FP (ºC) Table 9: Flash pont of mxtures 2-propanol-ethylene glycol x FP (ºC) Table : Flash pont of mxtures sobutanol-ethylene glycol x FP (ºC) Table 11: Flash pont of mxtures 2-propanol-sobutanol x FP (ºC) RESULTS AND DISCUSSION The flash pont of a pure substance s acheved when ts partal pressure s equal to the lower flammablty lmt. In a general way, the flash pont of a flammable compound n a mxture, may be mathematcally expressed as equaton [1]: LFL P = γ x P, [1] Where LFL s the Lower Flammablty Lmt of, P s the total pressure of the sat system, γ s the actvty coeffcent of, x s the molar fracton of the lqud and P, FP s the saturaton pressure of at flash pont temperature. Equaton [1] s vald f there s only one flammable compound n the mxture (.e. bnary aqueous mxtures). In other cases, we must mprove the equaton, because t gves one flash pont condton for each flammable compound, and the mxture has only one flash pont. sat FP 3

4 The man problem s to gve a lower flammablty lmt representatve of the whole mxture. In ths way Le Chateler (1891), Prugh (1973) Hanley (1998) and Kanury (1983) have developed some methods and equatons whose accuracy have been tested n ths work. The second problem s to estmate the saturaton pressure. It s obvous that f we use better correlatons when estmatng the needed parameters, we wll obtan better results. The equatons of Antone and Clausus-Clapeyron have been selected to estmate the saturaton pressure. The parameters A, B and C for Antone s equaton and H v for Clausus-Clapeyron one, were obtaned from Polng et al. (2001), and Lde (1995). The thrd and last problem, and the worst, s the actvty coeffcent. If expermental data are avalable, fttng of them s always possble, but we usually don t have them. The best equatons, f we have expermental data, are that of Margules and that of Van Laar, and UNIFAC f we don t have them. As an example, we wll develop the equaton obtaned applyng the equatons of Antone and Margules, and Le Chateler s rule (1891): If temperature s under the flash pont: Then, usng the Le Chateler s rule, at the flash pont: y y < LFL < 1 [2] LFL y LFL From Dalton s and Raoult s laws: sat x P y = γ [4] P Substtutng the value of γ from Margules and P sat from Antone: = 1 [3] y ( x ( A + 2( A A ) x ) B A T + C exp 2 j j j j x = [5] P Where, j =1,2 ( j); A, B, C are the Antone s coeffcents for, and A j, A j are the Margules coeffcents for the bnary mxture consdered. Then, wth [3] and [5], makng T = FP: ( x ( A + 2( A A ) x ) B A FP+ C exp 2 j j j j x = 1 P LFL [6] 4

5 Solvng [6], we obtan the flash pont expected for the mxture. If we don t have the value of LFL, t may be calculated from FP and Antone s equaton: A B 2 ( x ( A + 2( A A ) x ) B A FP+ C FP + C exp j j j j x LFL = ; = 1 [6.a] B P A FP + C Where FP s the flash pont of the pure compound. Smlar equatons have been tested to determne whch combnaton gves the best results. From our work, we have reached the concluson that a modfcaton of the equaton proposed by Prugh (1973), gves better results: LFL = a [7] C st Where a s a constant (Prugh gave a = 0.55) and C st s the theoretcal stochometrc concentraton of oxygen needed n the combuston of the molecule. After fttng wth more than 400 compounds, we have obtaned a better correlaton wth a = And the stochometrc concentraton s calculated as: C 83.8 = st 4 [8] ( C) + 4( S ) + ( H ) ( X ) 2( O) Where C, S, H, X and O are the numbers of the respectve element n the molecular formula of the compound (X means halogen). Better results are obtaned f the stochometrc concentraton of oxygen s calculated trough [9]: C = 0.21 st ( C) + ( S ) ( H ) 0.625( X ) 0.5( N ) 0. 5 ( O) [9] In table 12 a sample of our results for the mxture 1-propanol-water s shown. Table 12: Correlatons for 1-propanol-water MARGULES VAN LAAR UNIFAC x FP E FP(1) FP(2) FP(3) FP(4) FP(1) FP(2) FP(3) FP(4) FP(1) FP(2) FP(3) FP(4) (1): Hanley equaton + Antone equaton (3): Antone equaton + modfed Prugh (2): Antone equaton (4): Clausus-Clapeyron 5

6 The accuracy of the correlatons may be seen n fgures 1, 2 and 3. Expermental Hanley + Antone Antone Antone + Prugh Clausus-Clapeyron 60 FP (ºC) x (molar fracton) Fgure 1: Flash pont of 1-propanol-water mxtures. (Margules equaton for actvty coeffcents). Expermental Hanley + Antone Antone Antone + Prugh Clausus-Clapeyron 60 FP (ºC) x (molar fracton) Fgure 2: Flash pont of 1-propanol-water mxtures. (Van Laar equaton for actvty coeffcents). 6

7 Expermental Hanley + Antone Antone Antone + Prugh Clausus-Clapeyron 50 FP (ºC) x (molar fracton) 5. CONCLUSIONS Fgure 3: Flash pont of 1-propanol-water mxtures. (UNIFAC for actvty coeffcents). Once all the data have been analysed, the followng conclusons have been acheved: 1. All the hypothess gve equatons to estmate the flash pont of pure compounds and bnary mxtures accurately. The greater devatons are consequence of worse correlatons to estmate the actvty coeffcents. Specfcally: a) The saturaton pressure s better estmated trough Antone s equaton. Clausus- Clapeyron gves too hgh values for the flash pont. b) Margules and van Laar equatons gve approxmately the same accuracy. UNIFAC gves greater devatons. 2. Hanley s equaton and a modfcaton of Prough s equaton provde a smlar fttng to expermental data. 3. The best proposed method s that one whch use Antone s equaton for determnaton of the saturaton pressures and Margules or van Laar s equatons for determnaton the actvty coeffcents. The worst equaton s that whch use Clausus- Clapeyron s equaton for determnaton of the saturaton pressures and UNIFAC for determnaton of the actvty coeffcents. 7

8 6. BIBLIOGRAPHY FALBE, J., BAHRMANN, H., LIPPS, W. and MAYER, D., Alcohols, alphatc. In: F. Ullmann, ed. Ullmann s Encyclopeda of Industral Chemstry. 6 th ed. Wenhem: Wley-VCH, vol. 2, GMEHLING, J. and RASMUSSEN, P., Flash pont of flammable lqud mxtures usng UNIFAC. Ind Eng Chem Fund, 21 (2), HANLEY, B., A model for the calculaton and verfcaton of closed cup flash ponts for multcomponent mxtures. Process Safety Prog, 17 (2), KANURY, A.M., A relatonshp between the flash pont, bolng pont and the lean lmt of flammablty of lqud fuels. Combust Sc Technol, 31, LE CHATELIER, H., Estmaton of fredamp by flammablty lmts. Ann Mnes, 19 (8), LENOIR, J.M., Predct flash ponts accurately. Hdrocarb Process, 54 (1), LIAW, H.-J., CHIU, Y.-Y., The predcton of the flash pont for bnary aqueousorganc solutons. J Haz Mat, 1 (2), LIDE, D.R., Handbook of organc solvents. Boca Raton: CRC Press. MARTÍNEZ, P.J., RUS, E., COMPAÑA J.M., (2002). Determnaton of flash pont of mxtures between organc compounds and water. In: 9º Medterranean Congress of Chemcal Engneerng, Barcelona /02. 5/ PAPA, A.J. and SHERMAN, P.D., Ketones. In: KIRK, R.E. and OTHMER, D.F. eds. Encyclopeda of Chemcal Technology. 3 rd ed. New York: J. Wley, vol. 13, PARRISH, C.F., Solvents, ndustral. In: In: KIRK, R.E. and OTHMER, D.F. eds. Encyclopeda of Chemcal Technology. 3 rd ed. New York: J. Wley, vol. 21, POLING, B.E., PRAUSNITZ, J.M. and O CONNELL, J.P., The propertes of gases and lquds, chap. 7, 8 and Appendx. 5 th ed. New York: McGraw-Hll. PRUGH, R.W., Estmaton of Flash Pont Temperature. J Chem Educ, 50, A SIEGEL, H. and EGGERSDORFER, M., Ketones. In: F. Ullmann, ed. Ullmann s Encyclopeda of Industral Chemstry. 6 th ed. Wenhem: Wley-VCH, vol. 18, STOYE, D., Solvents. In: F. Ullmann, ed. Ullmann s Encyclopeda of Industral Chemstry. 6 th ed. Wenhem: Wley-VCH, vol.33, SUZUKI, T., OHTAGUCHI, K. and KOIDE, K., A method for estmatng flash pont of organca compounds from molecular structures. J Chem Eng Japan, 24 (2), WERLE, P. and MORAWIETZ, M., Alcohols, polyhydrc. In: F. Ullmann, ed. Ullmann s Encyclopeda of Industral Chemstry. 6 th ed. Wenhem: Wley-VCH, vol. 2,

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