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Thermal Stability of Acidic Sulfates in Krafi Recovery Bode

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Thermal Stability of Acidic Sulfates in Krafi Recovery Bode Recoverv Boiler Debosits Thermal stability of acidic sulfates in krafi recovery bode Honghi Tran, William Poon, and David Barham and severe tube wastage via corro- ABSTMCR Acidic sulfates, such us NuHS04 and Nu2S20?, sion (3-5). ure suspected in sticky depositformution und tube corrosion tn In previous work (6), it has been shown that forming 'sodium bisul- the generuting bunk and economizer regions of kru$ recovery fate (NaHSO,) directly from sodium boilers. Their stubility wus exumined in uir, moist conditions, sulfate (Na,SO,) or salt cake is both and in the presence ofNa2C03ut various temperutures. The kinetically and thermodynamically to feasible under boiler upset condi- results showed that, in uir, NuHSO, melts und decomposes tions that lead to high SO, levels in solid Nu2S207una? wuter vupor ut ubout 180 O C. Nu2S207is the flue gas. The reaction kinetics relutively stable up to its melting point of 380 C. Molten depend strongly on temperature and so SOJSO, and H,O concentrations in Nu2S207purtiully decomposes to lid Nu2S04,which reucts the gas phase. At 250qfor instance, with the remuining Nu2S207to form u newly identijed liquid NaHSO, forms readily if the compound, 3Nu2S,0;2Na2S04; this compound melts at SO, (SO, + SO,) concentration ex- its react ceeds 150 ppm. 570' C. Solid Nu2S207and complex compound rupidly In recovery boilers, the SO, con- with H20 vupor ut 300' C to reTom liquid NuHSO,, which centration in the flue gas rarely ex- cun be corrosive for the generuting bunk tubes during boiler ceeds 200 ppm. Therefore, the most operution. These ucidic sulfates can coexist with Nu2C03 below likely compound that makes depos- its acidic in recovery boilers is their respective melting points. They ure hygroscopic, u bsorbing NaHSO,, since it requires less than wuterfiom moist uir to&rm su&ric mid, which muy cuuse 10 ppm SOxto form as a solid phase tube wustuge during boiler outuges. and less than 200 ppm to be present as a liquid phase (2). While it may be KEYWORDS: Deposits, recovery firnuces, sodium carbonute, possible for solid sodium pyrosulfate (Na,S,O,) to form in recovery Coil- sulfates, temperature, thermal stability, wuter. ers, liquid Na,S,O, cannot be formed due to its requirement of high SO, levels, i.e., levels greater than 2500 ireside deposits on the generati ers burning high-sulfidity black li- ppm (7). For boilers that burn hard- Fing bank and economizer region quors or in those operating at low wood black liquor, the potassium con- tubes of kraft recovery boilers are bed temperatures (1,Z). Such acidic tent in the deposits may be high. occasionally acidic when dissolved in deposits may be responsible for both Therefore, potassium bisulfate water. This is more common in boil- fouling of heat transfer surfaces (1) (KHSO,) and potassium pyrosulfate (K$,O,) may be formed in the de- posits, since they require much lower SO, concentrations than the equiva- Tran is a professor and associate director of The Pulp and Paper Centre. Poon is a lent sodium salts (2, 7). graduate student and Barham is a professor at The Pulp and Paper Centre, Once formed, it is not known if Department of Chemcial Engineering and Applied Chemistry, University of Toronto, NaHSO, can remain stable during Toronto, ON M5S 1A4, Canada. 128 May 1994 Tappi Journal ing samples of NaHSO, and Na,S,O, to air with various relative humidi- ties for up to 18 and 21 days, respec- tively. Details of the experimental procedures can be found in Ref. 8. Results and discussion Thermal behavior of NaHSO, -20 1 i15 Figure P shows DTWI'GA results for NaHSO,. The four main endo- thermic events on the DTA curve beginning at 180'33, 240"C, 360"C, and about 400°C are each accompanied by a weight loss event on the TGA curve. The first thermal event is the -50k li0 IO0 3b0 4bO 5bO Si0 7bO 8k10 melting of NaHSO,. The third ther- TEMPERATURE, "C mal event is melting the mixture of NaHSO, and Na,S,O, formed by the partial decomposition of NaHSO, (Reaction l),and the fourth is the 1. X-ray diffraction data for the proposed Experimental procedures decomposition of Na,S,O, (Reaction new compound 3Na,S,0;2Na,S04 (CuKa 2). target, Ni filter) Samples of NaHSO, and Na,S,O, were subjected to increasing-tem- 2NaHSO,(l) + Na,S,O,(s) + 2H,O(g) 29, d value, l/lo perature simultaneous DTNTGA (1) deg A x 100 (differential thermal analysis/ thermogravimetric analysis) in a 12.83 6.90 15 Seiko Thermal Analyzer to investi- Na,S,O,(l) + Na,SO,(s) + SO&) (2) 18.35 4.84 18 19.63 4.52 17 gate their thermal stabilities. In Note that while the total decom- 21.30 4.17 38 DTA, the temperature difference position of NaHSO, to Na,SO, should 25.79 3.45 17 between a reactive sample (e.g., give a theoretical weight loss of 27.56 3.24 29 NaHSO,) and a thermally inert stan- 40.8%, the experimental maximum 28.58 3.12 100 dard (e.g., Al,O,) is plotted against value is only about 38%. This is be- 32.17 2.78 13 temperature. Any temperature dif- cause the original NaHSO, contained ference is related to a thermal event, a small amount (about 6 wt%) of such as melting or decomposition, in Na,SO,. The presence of Na,SO, normal boiler operation; thermody- the sample. In TGA, a plot of weight probably also accounts for the sec- namically it cannot. Furthermore, change vs. temperature for the ond thermal event, which is likely to since deposits usually contain some sample can also be used to identify a be a eutectic melting point in the sodium carbonate (Na,CO,), which is thermal event in the sample. ternary system NaHS0,-Na,S,O,- alkaline, it is questionable whether Separate isothermal (constant Na,SO,. Note also that the decompo- NaHSO, and Na,S,O, can be formed temperature) TGA experiments were sition of NaHSO, after it begins to and be stable in such deposits. performed on both compounds in air melt at 180°C is slow, and that the The present study examines the for time periods from ten minutes to decomposition of Na,S,O, also slows thermal and kinetic behavior of both as long as two months, depending on at about 480°C. Both of these obser- NaHSO, and Na,S,O, in air at high the experimental temperature. The vations suggest that the material re- temperatures. The effects of Na,CO, effect of Na,CO, on the stability of solidifies as it decomposes or that a and H,O vapor on the stability of these acidic sulfates was also exam- solid intermediate compound is these acidic sulfates at various tem- ined by subjecting mixtures of formed. peratures are also examined to make NaHSO, and Na,CO, (2:l molar ra- Figures 2-4 show isothermal TGA the study more applicable to actual tio), and Na,S,O, and Na,CO, (1:l results for NaHSO, heated in air. In kraft recovery boiler conditions. molar ratio), to isothermal TGA. The Fig. 2, the decomposition of NaHSO, stability of acidic sulfates in moist to Na,S,O, at 250 and 300°C occurs atmospheres was studied by expos- rapidly with a weight loss of 7.5%, Vol. 77, No. 5 Tappi Journal 129 2. Isothermal TGA of NaHSO, in air at 250-350°C 3. Isothermal TGA of NaHSO, in air at 400-550°C 0, -1I I Or----- 1 250°C 300°C -1 5 -350°C -25 -20 1 -300L' .A 10 20 30 40 50 60 70 -50; 5 10 15 20 25 30 35 4( TIME, days TIME, h -~ ~ - I 4. Isothermal TGA of NaHSO, in air at 600-800°C 5. Time for total NaHSO, decomposition at various temperatures in A I 2.5 - 1 I.iooac -500 a- 12345676 TIME, h TEMPERATURE, "C but the decomposition to Na,SO,, relatively stable compound between Figs. 24,vs. temperature. The peak with a theoretical total weight loss of the Na,S,O, and Na,SO, from the at 550°C again suggests the pres- 40.8%, does not occur in any reason- sequential decompositionof NaHSO, ence of a relatively stable compound able time. This is also shown by the and Na,S,O,. Similar results are containing Na,S,O, and Na,SO,. 350°C curve. The curves in Fig. 3 are shown for the test at 600°C (Fig. 4). somewhat puzzling unless the results Calculations based on weight loss Thermal behavior of Na2S,O7 from Figs. 1 and 2 are considered at show that this formerly unknown Figure 6 shows DTA/TGA results the same time. As the temperature compound is likely to be 3Na,S,O, for Na,S,O, heated in air at an in- is increased from 400°C to' 550"C, the .2Na,SO,. It shows a completely dif- creasing temperature. The endother- long-term stability of the NaHSO, ferent X-ra,y diffraction (XRD) pat- mic peak at 270°C is probably due to' decomposition product increases. tern compared to other acidic sulfates the melting of an NaHSO, - Na,SO, The leveling-off of the 350°C curve (8). The major XRD peaks for the - Na,S,O, mixture. This is because (Fig. 2) and of the 450"C, 500"C, and new compound are given in Table I. the Na,S,O, used was made by dehy- 550°C curves (Fig. 3) at about 18% Figure 5 shows the time neces- drating NaHSO,, which contained weight loss is interesting.
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