CHEMICKÉ ROZPÚŠŤANIE PERIKLASU V ZRIEDENEJ HCL. Katedra keramiky, Hutnícka fakulta Technickej univerzity, Letná 9/A, Košice
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1 Aa Meallurgia Slovaa, 1, 6, ( - 8) CHEMICKÉ ROZPÚŠŤANIE PERIKLASU V ZRIEDENEJ HCL Fedoročková A. 1, Rashman P. 1 Kaedra hémie, Huníka fakula Tehnikej univerziy, Lená 9/A, Košie Kaedra keramiky, Huníka fakula Tehnikej univerziy, Lená 9/A, Košie CHEMICAL DISSOLUTION OF PERICLASE IN DILUTE HYDROCHLORIC ACID Fedoročková A. 1, Rashman P. 1 Deparmen of Chemisry, Fauly of Meallurgy, Tehnial Univerziy of Košie, Lená 9/A Deparmen of Ceramis, Fauly of Meallurgy, Tehnial Univerziy of Košie, Lená 9/A Absra Kineis of he reaion beween pariulae polyrysalline and dilue hydrohlori aid were sudied wih speial regard o he rae and mehanisms of hemial dissoluion of. The effe of proess parameers viz. onenraion of H + ions, emperaure and parile size was invesigaed. I was observed ha he rae of ransfer of magnesium o he soluion: a) inreased wih inrease in boh HCl onenraion (from 1 - M o 1-4 M) and emperaure (from 5 C o 6 C); b) dereased wih inrease in parile size (from 63 o 355 µm). To obain he emperaure and onenraion dependene of he rae of perilase dissoluion, onversion vs. ime daa measured a differen emperaure and differen iniial ph of he soluion were analysed. I was onluded ha rae of dissoluion dereased wih inreasing ph over he whole emperaure range onsidered in he presen work (5 C 6 C). Sine he slope of log (rae) vs. ph urve an provide a useful informaion on he mehanism dissoluion (naure of he rae deermining sep), he slope values were alulaed for individual experimens. Even hough obained values (,16 < n <,91) are, wihin an experimenal error, onsisen wih lassi kinei heories (Vermilyea, Diggle, Gorihev), he rae-onrolling sep ould no have been assigned unambiguously. Nonlinear shape of he urve log r = f(ph) indiaes ha rae-deermining seps of differen naure may our a differen ph, or ha individual effes of various rae-deermining seps an be hanged as ph is hanged. We onlude ha a ph, he rae is probably onrolled by he proonaion of he O - ions o OH - (O +H + OH - ). A higher ph values, he rae an be onrolled eiher by proonaion of surfae hydroxyl groups (OH - + H + H O) or peneraion of proons under he surfae of he solid phase. A higher emperaure and ph 4, proonaion of O - ions o form a waer moleule (O - + H + H O) or ranspor of + ions from he solid surfae beome probably he rae deermining seps. Key words: Magnesium oxide; Hydrohlori aid; Chemial dissoluion; Rae; Mehanism Absrak Práa sa zaoberá experimenálnym šúdiom vplyvu konenráie, eploy a granulomerie na kineiku hemikého rozpúšťania syneikého periklasu v zriedenej kyseline hlorovodíkovej. V oblasi použiýh reakčnýh podmienok sa zisilo, že rýhlosť rozpúšťania : a) rasie ak so zvyšujúou sa konenráiou kyseliny hlorovodíkovej (1 - M M), ako aj s rasúou eploou (5 C 6 C); b) klesá s rasúim rozmerom časí ( µm).
2 Aa Meallurgia Slovaa, 1, 6, ( - 8) 3 Z nameranýh priebehov časovýh závislosí konverzie horčíka pri rôznyh eploáh a počiaočnýh konenráiáh HCl (ph) bola vyhodnoená eploná závislosť rýhlosi rozpúšťania. Bolo zisené, že rýhlosť rozpúšťania klesá s rasúim ph v elom sledovanom rozsahu eplô. Pre ďalšie úvahy o mehanizme rozpúšťania bolo účelné (v súlade s kineikými eóriami) odhadnúť hodnou smernie závislosi log r ph. Aj napriek omu, že experimenálne určené hodnoy smerní sa pohybujú v inervale,16 < n <,91, korý je v rámi experimenálnyh hýb v súlade s predpoveďami klasikýh eórií (Vermilyea, Diggle, Gorihev), nie je možné na ih základe jednoznačne priradiť riadiai dej alebo poukazujú na úplne odlišné mehanizmy riadenia. Nelineárny priebeh závislosi log r = f(ph) navyše signalizuje, že so zmenou ph v ejo oblasi dohádza k zmene riadiaeho deja, resp. že sa miera vplyvu rôznyh riadiaih dejov mení. Podľa eórie môže byť riadiaim krokom v oblasi ph povrhová hydroxyláia (O - +H + OH - ). S nárasom ph môže úlohu riadiaeho deja posupne preberať proonáia hydroxylovýh skupín (OH - + H + H O), prípadne podpovrhová peneráia proónov. Výsledky naznačujú, že pri vyššíh eploáh a ph 4 sa ako rýhlosť určujúi krok môže uplaniť buď jednosupňová proonáia (O - + H + H O) alebo odsraňovanie kaiónov + z povrhu oxidu. 1. Úvod Šúdium kineiky hemikého rozpúšťania oxidov v kyselináh je problemaikou, korej aplikáie spadajú do veľmi širokej oblasi proesov, počnú environmenálnymi a geohemikými proesmi, ez koróziu, kaalýzu až k priemyselnej výrobe liečiv. Aj napriek omu, že za poslednýh ridsať rokov bol na úo ému publikovaný elý rad prehľadnýh prá [1-5], súhrne sa o nih dá povedať, že sú veľmi heerogénne ak prísupom k danej problemaike, rozsahom reakčnýh podmienok ako aj formulovanými závermi. Kineike hemikého rozpúšťania periklasu () bola venovaná pomerne veľká pozornosť. Rôzni auori zisili, že rozpúšťanie môže prebiehať v difúznej alebo kineikej oblasi, j. elková rýhlosť proesu môže byť v závislosi od reakčnýh podmienok určená rýhlosťou difúzie kvapalnýh reakanov a/alebo produkov, resp. povrhovou reakiou [4-11]. Hlavným problémom pri šúdiu mehanizmu však je skuočnosť, že exisuje viaero eórií, korýh použiie vedie niekedy k rôznym záverom a neumožňuje jednoznačne určiť riadiai dej [,1,13]. Navyše sa posupne objavujú aj režimy, koré sa pomoou jesvujúih kineikýh eórií nedajú vysveliť [,8,14]. Tieo skuočnosi naznačujú, že formulovanie všeobenýh zákoniosí, korými sa riadi hemiké rozpúšťanie periklasu, si vyžaduje ak dôkladné experimenálne šúdium správania sa v širokom inervale reakčnýh podmienok, ako aj kriiké prehodnoenie exisujúih eórií. Cieľom ejo práe je: a) doplniť a rozšíriť doposiaľ publikované informáie o rýhlosi rozpúšťania o údaje namerané pri vyššíh eploáh b) analyzovať vzťah medzi mehanizmom a reakčnými podmienkami na základe doeraz publikovanýh eórií popisujúih hemiké rozpúšťanie.. Experimenálna časť.1 Použié maeriály Vplyv reakčnýh podmienok na kineiku lúhovania bol sledovaný na roh zrniosnýh riedah vysokočisého produku hemikého spraovania magneziovýh úleov
3 Aa Meallurgia Slovaa, 1, 6, ( - 8) 4 závodu Hačava (HAMAG). Predúprava vzoriek bola uskuočnená mleím a suhým riedením na siáh. V snahe vyhnúť sa hybám, koré môže spôsobiť prípadná príomnosť veľmi malýh časí, nalepenýh na povrhu väčšíh počas mleia, boli vzorky po mleí a riedení na siáh premyé aeónom a opäovne presiované. Fyzikálno-hemiké harakerisiky použiýh vzoriek sú uvedené v abuľke 1. Lúhovaím činidlom bola kyselina hlorovodíková p.a. (35 hm.%), riedená podľa poreby desilovanou vodou. Table 1 Physio-hemial haraerisis of samples of perilase HAM/67 HAM/113 HAM/335 Parile diameer [µm] Mean parile diameer [µm] Speifi surfae area [m.g -1 ] Chemial omposiion w i [%] 99.5 CaO.15 Fe O 3.1 Al O 3. SiO.4 L.O.I <.1 Raional analysis w i [%] perilase () 99.5 magnesiumferrie (.Fe O 3 ).6 dialiumsiliae (CaO.SiO ).1 brownmillerie (4CaO.Al O 3.Fe O 3 ).1 dialiumferrie (CaO.Fe O 3 ).8. Použié meódy Kineiké merania boli uskuočnené v laboraórnom izoermikom miešanom reakore. Vlasný miešaný reakor vorí sklenená valoviá nádoba s elkovým objemom 1,5 dm 3, vybavená vruľovým miešadlom a 4 bočnými zarážkami. Izoermiký priebeh meraní bol zabezpečený pomoou emperovaieho hada spojeného s ermosaom. Rozsah hemikej reakie bol určený na základe koninuálneho merania zmeny ph ( ph) v reakčnej zmesi, v korej prebieha rozpúšťanie. Do reakora prepojeného s ph-merom (Mikroehna, M 1) bola nadávkovaná kyselina hlorovodíková (nižšej konenráie ako zodpovedá požadovanej počiaočnej hodnoe ph), reakor bol uzavreý, napojený na ermosa a za sáleho miešania vyemperovaný na sanovenú eplou s presnosťou ±,1 K. Po dosiahnuí reakčnej eploy bola niekoľkými kvapkami HCl nasavená počiaočná hodnoa ph rozoku (ph ) na požadovanú hodnou a objem upravený na V (V =,8 dm 3 ). V čase = bola do reakora nadávkovaná vzorka syneikej magnézie (m ). Úbyok konenráie vodíkovýh iónov bol snímaný kombinovanou sklenenou elekródou (Thea 9, HC 13) kalibrovanou na kalibračné rozoky Tirisol (Merk) v oblasi, zodpovedajúej zmene ph pri danýh reakčnýh podmienkah. Supeň konverzie bol vypočíaný na základe sehiomerie reakie podľa vzťahu (1) pri V = konš.: X H b H b H b ph ph + M V ( 1 1 ) () = = = = + + n V m, (1)
4 Aa Meallurgia Slovaa, 1, 6, ( - 8) 5 v korom H + b označuje zmenu konenráie H + iónov v objeme kvapaliny, +, + H b H b vyjadrujú počiaočnú konenráiu H + iónov a ih konenráiu v čase, m je navážka vzorky magnézie. Podmienky merania boli volené ak, aby záznam umožnil vyhodnoenie časovej závislosi konverzie slinku v priebehu lúhovania s požadovanou ilivosťou,.j. aby zreagované množsvo slinku v počiaočnýh šádiáh rozpúšťania (X < 1%) vyvolalo zmenu ph rádovo vyššiu ako je ilivosť ph-mera. 3. Výsledky Rýhlosť rozpúšťania vzoriek HAM/67, HAM/113, HAM/335 bola šudovaná pri počiaočnýh hodnoáh ph =, 3 a 4 v eplonom inervale 5 C až 6 C. Vplyv eploy na časový priebeh konverzie bol sledovaný pri roh počiaočnýh konenráiáh HCl v eplonom inervale 5 C 6 C. Priebeh kineikýh kriviek na obr.1 dokumenuje ilivú odozvu rýhlosi rozpúšťania na rasúu eplou.,1,8 X,6,4, 5 C 45 C 6 C [min] Fig.1 Effe of emperaure on fraion of dissolved (HAM/113; HCl=.1 M) Urýhľujúi vplyv eploy bol zaznamenaný aj pri rozpúšťaní syneikej magnézie v zriedenejšej kyseline (ph =3 a 4). Pri šúdiu vplyvu konenráie sa zisilo, že rýhlosť rozpúšťania horčíka klesá s klesajúou konenráiou HCl (nárasom ph). Siuáia je pri eploe 5 C znázornená na obr.. Analogiký priebeh bol pozorovaný aj pri 45 C a 6 C. X,1,8,6,4 ph = ph = 3, ph = [min] Fig. Effe of hydrohlori aid onenraion on fraion of dissolved (HAM/113; ϑ = 5 C)
5 Aa Meallurgia Slovaa, 1, 6, ( - 8) 6 Okrem eploy a ph bol esovaný aj vplyv veľkosi časí. Z meraní vyplynulo, že rýhlosť rozpúšťania súpa s klesajúim rozmerom časí. Siuáiu ilusruje obrázok 3. X,1,8,6,4, [min] Fig.3 Effe of parile size on fraion of dissolved ( HCl =.1 M; ϑ = 5 C) 4. Diskusia a závery Pri vyhodnoovaní meraní ph sme vyhádzali z predpokladu, že povrhová ploha časí a eda aj rýhlosť rozpúšťania v počiaočnom šádiu proesu (.j. pri X,1, čo zodpovedá ph,4) je prakiky konšanná. Na základe uvedenýh predpokladov plaí vzťah (): r.. S. M m m () kde r rýhlosť rozpúšťania, reakčný čas, S elková ploha povrhu časí vo vzorke, M mólová hmonosť, m navážka vzorky, j. hmonosť pred rozpúšťaním, m hmonosť nezreagovaného v čase. Úpravou vzťahu () získame rovniu (3): X ( ) r. S. M. = k = (3) A. kde je konšana ( k = r. S A M [s -1 ]). Hodnoy počiaočnýh rýhlosí rozpúšťania sme získali lineárnou regresiou nameranýh údajov (aspoň roh paralelnýh pokusov) pomoou vzťahov (1) a (3). Výsledky sú uvedené v abuľke. k Table Iniial raes of dissoluion ph = ph = 3 ph = 4 Temperaure [ C] r log r r log r r log r 5 1.4x x x x x x x x x Z priebehov závislosí X - pri rôznyh eploáh a počiaočnýh konenráiáh HCl (rôznyh ph ) bola vyhodnoená eploná závislosť rýhlosi rozpúšťania. Obrázok 4
6 Aa Meallurgia Slovaa, 1, 6, ( - 8) 7 ukazuje, že rýhlosť rozpúšťania klesá s rasúim ph v elom sledovanom rozsahu eplô. Vplyv eploy je najvýraznejší pri ph a s rasúim ph klesá. -3 log r -3,5-4 -4,5-5 -5,5 5 C 45 C 6 C ph Fig.4 Temperaure dependene of log r = f(ph ) for HAM/113 Pre ďalšie úvahy o mehanizme rozpúšťania je účelné (v súlade s kineikými eóriami [, 1, 13]) odhadnúť hodnou smernie závislosi log r ph. Výsledky uvádza abuľka 3. Table 3 Calulaed values of he slopes of log (rae) vs. ph dependene Calulaed values ph - n = d log r dph 5 C 45 C 6 C 3 (1) () (1) (1) value alulaed as (log r log r 1 )/(ph ph 1 ) () value obained by a nonlinear regression of log r vs. ph dependene Z hodnô v ab.3 vyplýva, že pri rozpúšťaní v zriedenýh rozokoh HCl smernia závislosi log r ph pri každej eploe klesá so zvyšujúim sa ph. Určené hodnoy smerní sa pohybujú v inervale,16 < n <,91, korý je v rámi experimenálnyh hýb v súlade s predpoveďami klasikýh eórií (Gorihev [],Vermilyea [1], Diggle [13]). Nelineárny priebeh závislosi log r = f( ph) navyše signalizuje, že so zmenou ph v ejo oblasi dohádza k zmene riadiaeho deja, resp. že sa miera vplyvu rôznyh riadiaih dejov mení. Podľa eórie môže byť riadiaim krokom v oblasi ph povrhová hydroxyláia (O +H + OH - [13]). S nárasom ph môže úlohu riadiaeho deja posupne preberať proonáia hydroxylovýh skupín (OH - + H + H O [1,13]), prípadne podpovrhová peneráia proónov []. Pri vyššíh eploáh a ph 4 sa ako rýhlosť určujúi krok môže uplaniť buď jednosupňová proonáia (O - + H + H O [1,13]) alebo odsraňovanie kaiónov + z povrhu oxidu [13]. Poďakovanie Táo práa bola podporená Vedekou granovou agenúrou MŠ SR a SAV (Gran 1/36/6)
7 Aa Meallurgia Slovaa, 1, 6, ( - 8) 8 Lieraúra [1] Warren I.H., Devuys E.: Leahing of meal oxides. In: Evans D.J.I., Shoemaker R.S. (Eds.). Inernaional Symposium on Hydromeallurgy, AIMMPE, New York (1973) 9 [] Gorihev I. G., Kyprianov N. A.: Regular kinei feaures on he dissoluion of meal oxides in aidi media, Russ. Chem. Rev. 53 (1984) 139 [3] Summ W.: Aquai Surfae Chemisry: Chemial Proesses a he Parile-Waer Inerfae, John Wiley&Sons, New York 1987 [4] Segall R. L., Smar R. S. C., Turner P. S.: Oxide surfae in soluion. In.: Nowony, J., Dufour, L.C. (ed.), Surfae and Near-Surfae Chemisry of Oxide Maerials, Elsevier, Amserdam 1988 [5] Blesa M. A., Morando P. J., Regazzoni A. E.: Chemial Dissoluion of Meal Oxides, CRC Press, Florida 1994 [6] Vermilyea D. A.: Dissoluion of and (OH) in aqueous soluions, J. Elerohem. So., 116 (1969) 1179 [7] Segall R. L., Smar R. S. C., Turner P. S.: Ioni oxides: Disinion beween mehanisms and surfae roughening effes in he dissoluion of magnesium oxide, J. Chem. So. Faraday I 74 (1978) 97 [8] Jones C. F., Segall R. L., Smar R. S. C., Turner P. S.: Iniial dissoluion kineis of ioni oxides, Pro. Roy. So. Lond. A, 374 (1981) 141 [9] Fruhwirh O., Herzog G. W., Hollerer I., Raei A.: Dissoluion and hydraaion kineis of, Surf. Tehnol., 4 (1985) 31 [1] Wogelius R. A., Refson K., Fraser D. G., Grime G. W., Goff J. P.: Perifase surfae hydroxylaion during dissoluion, Geohimia e Cosmohimia Aa, 59 (1995) 1875 [11] Jordan G., Higgins S. R., Eggleson C. M.: Dissoluion of he perilase (1) surfae: A sanning fore mirosope sudy, Amerian Mineralogis, 84 (1999) 144 [1] Vermilyea D. A.: The dissoluion of ioni omponens in aqueous media, J. Elerohem. So., 113 (1966) 167 [13] Diggle J. W.: Dissoluion of Oxide Phases. In: Diggle, J.W. (ed.), Oxides and Oxide Films, Marel Dekker, New York 1973, 81 [14] Rashman P., Fedoročková A.: Sudy of inhibiing effe of aid onenraion on he dissoluion rae of magnesium oxide during he leahing of dead-burned magnesie. Hydromeallurgy, 71 (4) 43
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