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Corrosion Resistance of Selected Ceramic Materials to Sulfuric Acid

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Corrosion Resistance of Selected Ceramic Materials to Sulfuric Acid PLEASE 00 NOT REMOVE FRQ\1 LIBRARY I 9011 iRIi I Bureau of Mines Report of Investigations/1986 Corrosion Resistance of Selected Ceramic Materials to Sulfuric Acid By James P. Bennett UNITED STATES DEPARTMENT OF THE INTERIOR Report of Investigations 9011 Corrosion Resistance of Selected Ceramic Materials to Sulfuric Acid By James P. Bennett UNITED STATES DEPARTMENT OF THE INTERIOR Donald Paul Hodel, Secretary BUREAU OF MINES Robert C. Horton, Director Research at the Tuscaloosa Research Center is carried out under a memorandum of agreement between the University of Alabama and the Bureau of Mines. Library of Congress Cataloging in Publication Data: Bennett, James P (James Philip), 1951· Corrosion resistance of selected ceramic materials to sulfuric acid. (Bureau of Mines report of investigations; 9011) Bibliography: p. 11. Supt. of Docs. 110.: 128.23: 9011. 1. Ceramic materials-Corrosion. 2. Sulphuric acid. !. Title. II. Series: Report of investigations (United States. Bureau of Mines) ; 9011. TN23. U43 (TA430] 622s [620,1'404223] 85-600348 CONTENTS Abstract................ ....... .... ..•.... .. .. ...•... .. ...•.... ...•.... ........ 1 Introduction •....•....•.......•..•••........•......•.........•.......... 1-'" • •• 2 Test eq.uipment and sample description •••••••••••••••••••••••••• ,..... • •••• •••• • • 2 Results and discussion......................................................... 4 Acidproof materials.......................................................... 4 Acid-resistant materials................. ...... ... ..... .. ..... ....... ..... 7 Conclusions.................................................................... 10 References •••..•••..• '·e........................................................ 11 ILLUSTRATIONS 1. Construction detail of reaction vessel ••••••.•...••.•.••••••.••••.••••••••. 4 2. Total ions leached from acidproof materials in 110 days of H2S04 exposure •• 7 3. Total ions leached from acid-resistant materials in 110 days of H2S04 exposure. ... ... .. ...... .... ... .... .... ..... ..•.. .••. ...•... .. ... ... 10 TABLES 1. Chemical and physical properties of commercial ceramic materials ••••••••••• 3 2. Changes in weight of acidproof materials exposed to H2S04 for 110 days ••••• 5 3. Cold crushing strength of acidproof materials exposed to H2S04 for 110 days 5 4. Ions leached in 110 days from acidproof materials •••••••••••••••••••••••••• 6 5. Changes in weight of acid-resistant materials exposed to H2S04 for 110 days 8 6. Cold crushing strength of acid-resistant materials exposed to H2S04 for 110 days .•........•...•...•...••.•..•.....•............................ 1; • Q •••• 8 7. Ions leached in 110 days from acid-resistant materials ••••••••••••••••••••• 9 UNIT OF MEASURE ABBREVIATIONS USED IN THIS REPORT °c degree Celsius min minute 3 g/cm gram per cubic centimeter mm millimeter , ) h hour pct percent in inch psi pound per square inch L liter wt pct weight percent CORROSION RESISTANCE OF SELECTED CERAMIC MATERIALS TO SULFURIC ACID By James P. Bennett 1 ABSTRACT The Bureau of Mines is investigating the acid resistance of ceramic materials to identify construction materials for emerging technology in chemical and metallurgical processes. Eight commercial ceramic materi­ als, were evaluated: two red shale, two fireclay, one silicon carbide, one silica, one carbon, and one high-alumina. Samples were exposed to 10 wt pct H2S04 at 50° C and 10, 30, 50, 70, and 90 wt pct H2S04 at 90° C for time periods of 110 days. Statistically significant changes in cold crushing strength were observed in the silicon carbide and car­ bon materials. Weight changes and the leach rate of Al, Ca. Fe. K, Mg, Na. Si, and Ti were also monitored. The most severe corrosion conditions were at 90° C and 30 to 50 wt pct H2S04 for the acidproof and at 10 wt pct H2S04 for the acid-resistant materials. The silica and the high-alumina materials were the most acid-resistant, followed by the higher density red shale and fireclay. 1ceramic engineer, Tuscaloosa Research Center, Bureau of Mines, Tuscaloosa, AL. 2 BACKGROUND Extensive literature, published during Ammonium thiocyanate, for example, re­ recent years, identifies three gen­ sulted in much higher reaction rates with eral methods of fine-particle prepara­ boric acid in the BN synthesis (14). tion (1):2 (1) solution techniques, (2) Among the less conventional laboratory vapor-phase techniques, and (3) salt de­ techniques reported for the preparation composition techniques. Solution tech­ of nonoxide ceramic powders are the niques, also referred to as "chemical" reaction of compounds (sucr as silanes, preparation (2), offer the advantages of boranes, and halides) containing the de­ ease of preparation, good control of com­ sired cations in super-high-frequency position, and homogeneity. Among the so­ discharge plasma (15), chemical vapor lution techniques a number of terms, such deposition techniqueS:- (16-22), and the as "codecomposition" (3). "evaporative use of laser energy (~)-.-:Similar reac­ decomposition from solutions" (EDS) (4- tions have also been studied employing 5), "citrate process" (6). and "alkoxlde conventional high-temperature furnaces at process" (7) are frequently encountered. 1,5000 to 1,900° C (24-27). Vapor-phase techniques are receiving Production of complex: nitride powder more and more attention, due mostly to has been studied by the nitridation of interest in high-performance structural metal halides (SiCI4 , BCI3) in an N plas­ ceramics such as SiC and Si3N4. These ma (15). Chemical vapor deposition tech­ techniques lead to unaggreg~ted powders. niques have also been used to prepare Among the techniques in this category are thin films of BN, Si3N4, and TiN (8-12). all plasma methods (8-9) and others in­ Extremely fine, uniform Si3N4 and :SiC volving gaseous reactants. powders have been synthesized from SiH4, Decomposition of precursor salts (e.g., NH3, and CZH4 gas-phase reactants heated oxalates) has been employed in the prep­ by a COz laser (23). Nitrides of Si, B, aration of fine-powder carbides (10-11). and Ti have also De en prepared by the re­ BN powders have been prepared--by-the action of their halides with ammonia or reaction of boron oxides and borates with ammonia salts at high temperatures 24- ammonium chloride (NH4CI) in NZ and NH3 27). atmospheres (12). In certain reactions. --No mention of preparing BN from halides in order to increase the reaction rates of B with the reaction of ammonia salts in the solid state, that is, to effec­ or ammonia in the liquid phase has been tively increase the reaction surface ar­ made in the literature. In view of this eas, inert fillers such as CaC03 and cal­ finding, research efforts included a cium phosphates have also been employed study of obtaining ultrafine BN powders (13). Ammonium salts other than NH4CI from the reactions of halides with NH4Cl have also been used in BN synthesis. and NH3 in the liquid phase. EXPERIMENTAL EQUIPMENT AND PROCEDURES REACTIONS BETWEEN 5000 AND 750 0 C was used. Inorganic B compounds used in­ cluded boric oxide (Bz03), boric acid Two different approaches were eval­ (H3 B0 3), borax (Na2B407'10H:cO), and an­ uated for the synthesis of fine BN hydrous sodium tetraborate (Na2B407)' powders. The first was the reaction be­ Carbimide (NHZ"CO-NHZ) and thiocarbimide tween an inorganic B compound and an (NHzoSO'NHz) were used as N2 sources. organic N compound between 500 0 and 750 0 The powdered reactants were mixed in C in an NH3 atmosphere. For this a high­ stoichiometric proportions and placed in temperature controlled-atmosphere furnace the furnace. The furnace chamber was evacuated and purged with NH~ gas before 2Underlined numbers in parentheses re­ the temperature was raised. Experiments fer to items in the list of references at ran from 4 to 24 h at 500 0 to 750 0 C. the end of this report. 3 REACTIONS BETWEEN -750 AND 2000 C containing less than 1 ppm 02 and/or moisture. This high-purity inert atmos­ The second approach involved the syn­ phere was obtained by circulating the gas thesis of BN through reactions between in a closed system going through a puri­ various Nand B compounds leading to the fying chamber equipped with molecular formation of PQssible elemento-organic sieves to trap 02 and moisture. Figure 2 compounds as intermediate precursor spe­ shows the dry-box assembly. Reactions cies, the decomposition of which might were carried out in the experimental unit lead to BN formation. Such compounds (fig. 3) consisting of· a three-necked, included NH3, boron halides (principal­ 500-mL glass reaction vessel and a small ly boron trichloride, BC13), ammonium vacuum system with cold traps. chloride (NH4Cl), and sodium borohydride Three systems were studied. They in­ ( NaBH4)' cluded ammonia-boron halide, ammonium For the second approach, material salt-boron halide, and ammonium salt­ preparation and handling procedures ~l1ere metal borohydride reactions. performed in a dry-box system, a simpli­ fied schematic of which is shown in fig­ to specific products does ure 1. Ihe atmosphere in the box was not imply endorsement by the Bureau of maintained by a VAC Dri-train3 unit capa­ Mines. ble of generating an inert gas atmosphere Glove PrellSure sensln, o Wat.r~_~==r-.,..j Purifier refill In 1----" EXHAUST Pressure control Vacuu Foot pedal Inerf Com ressed air gas Purifier Regeneration purge Control panel a d vaouum subassembly Regeneration ur e as (valve ponol) Dri - train oontrol panel Compressed air Regeneration purge gall (60 to 100 psi) 3 to 10 pot HI!
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