烧结法制备炭黑/铝酸钙水泥及其结合耐火浇注料的性能
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摘要
以氧化铝、氧化钙及炭黑为原料,聚乙烯吡咯烷酮(PVP)水溶液为分散剂,经球磨混合、干燥、压坯,通过埋碳烧结法制备炭黑/铝酸钙水泥(CCAC)。利用X射线衍射仪、扫描电子显微镜和能谱仪研究了PVP水溶液浓度对产物物相组成和显微结构的影响;并分别通过沉降实验和综合热分析研究了炭黑/铝酸钙水泥的水润湿性和抗氧化性。结果表明:5%(质量分数)PVP的添加可以使炭黑的Zeta电位从–22.4 m V下降到–34.4 m V,炭黑在水中的分散性明显改善;经1 400℃保温4 h烧结后,5%PVP试样炭黑分布最均匀,产物中Ca O·Al_2O_3和CaO·2Al_2O_3的含量与商用Secar71水泥物相组成相近。与机械混合法制备的炭黑/铝酸钙水泥(S71CB)相比,埋碳烧结法制备的炭黑/铝酸钙水泥(CCAC–5,PVP水溶液浓度5%)具有较好的水分散性和抗氧化性。分别以S71CB和CCAC–5为结合剂制备刚玉质浇注料,研究了2种浇注料的力学性能和抗渣侵蚀性,结果表明:CCAC–5结合浇注料1 500℃烧结3 h后耐压强度和抗折强度分别比S71CB结合浇注料提高8.39%和10.71%,熔渣侵蚀率降低7%。CCAC–5结合浇注料表现出较好的力学和抗渣侵蚀性能,有望成为含碳浇注料的新型结合剂。
Carbon black/calcium aluminate cement(CCAC)was prepared by ball-milling mixing,drying and carbon-bed sintering with Al_2O_3,CaO and carbon black as raw materials,polyvinylpyrrolidone(PVP)as a dispersant.The effect of PVP concentration in aqueous solution on the phase composition and microstructure of the products was investigated by X-ray diffraction,scanning electron microscopy and energy dispersive spectrometry.The wettability and oxidation resistance of carbon black/calcium aluminate cement were analyzed by sedimentation and thermogravimetry–differential scanning calorimetry,respectively.The results show that the dispersibility of carbon black in water can be improved at 5%(in mass fraction)PVP.The Zeta potential decreases from–22.4 m V to–34.4 m V.After sintering at 1 400℃for 4 h,the distribution of carbon black in the sample with 5%PVP is uniform,the content of Ca O·Al_2O_3 and Ca O·2Al_2O_3(CA_2)in the product is similar to that of commercial cement Secar71.It is indicated that the carbon black/calcium aluminate cement(CCAC–5,PVP concentration of 5%)prepared by carbon-bed sintering has better water dispersibility and oxidation resistance,compared to the carbon black/Secar71(S71CB)prepared by mechanical mixing.Furthermore,the mechanical properties and slag corrosion resistance of corundum-based castables bonded with CCAC and S71CB,respectively,were compared.The cold crushing strength and cold modulus of rupture values of the castables bonded with CCAC–5 after fired at 1 500℃for 3 h are increased by 8.39%and 10.71%,respectively,and the slag erosion rate is decreased by 7%,compared to the castables bonded with S71CB.CCAC–5 shows good mechanical and slag corrosion resistance,as a promising binder for carbon-containing castables.
Carbon black/calcium aluminate cement(CCAC)was prepared by ball-milling mixing,drying and carbon-bed sintering with Al_2O_3,CaO and carbon black as raw materials,polyvinylpyrrolidone(PVP)as a dispersant.The effect of PVP concentration in aqueous solution on the phase composition and microstructure of the products was investigated by X-ray diffraction,scanning electron microscopy and energy dispersive spectrometry.The wettability and oxidation resistance of carbon black/calcium aluminate cement were analyzed by sedimentation and thermogravimetry–differential scanning calorimetry,respectively.The results show that the dispersibility of carbon black in water can be improved at 5%(in mass fraction)PVP.The Zeta potential decreases from–22.4 m V to–34.4 m V.After sintering at 1 400℃for 4 h,the distribution of carbon black in the sample with 5%PVP is uniform,the content of Ca O·Al_2O_3 and Ca O·2Al_2O_3(CA_2)in the product is similar to that of commercial cement Secar71.It is indicated that the carbon black/calcium aluminate cement(CCAC–5,PVP concentration of 5%)prepared by carbon-bed sintering has better water dispersibility and oxidation resistance,compared to the carbon black/Secar71(S71CB)prepared by mechanical mixing.Furthermore,the mechanical properties and slag corrosion resistance of corundum-based castables bonded with CCAC and S71CB,respectively,were compared.The cold crushing strength and cold modulus of rupture values of the castables bonded with CCAC–5 after fired at 1 500℃for 3 h are increased by 8.39%and 10.71%,respectively,and the slag erosion rate is decreased by 7%,compared to the castables bonded with S71CB.CCAC–5 shows good mechanical and slag corrosion resistance,as a promising binder for carbon-containing castables.
引文
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[20]DONNET J B,VOET A.Carbon black:physics,chemistry,and elastomer reinforcement[J].J Colloid Interf Sci,1977,62(1):195-196.
[21]高礼旋.炭黑的表面改性与包覆[D].广州:华南理工大学,2010.GAO Lixuan,Surface modification and encapsulation of carbon black(in Chinese,dissertation).Guangzhou:South China of Technology,2010.
[22]WANG Y,Li X,ZHU B,et al.Microstructure evolution during the heating process and its effect on the elastic properties of CAC-bonded alumina castables[J].Ceram Int,2016,42(9):11355-11362.
[23]DUTTA S,DAS P,DAS A,et al.Physical characteristics of alumina-carbon refractory castables containing calcium aluminate coated graphites[J].Inter Refract Man,2013,62(4):294-298.
[24]ZHANG J,JIA Q,YAN S,et al,Microstructure and properties of hydratable alumina bonded bauxite-andalusite based castables[J],Ceram Int,2016,42(1):310-316.
[2]LEE W E,VIEIRA W,ZHANG S,et al.Castable refractory concretes[J].Int Mater Rev,2001,46(3):145-167.
[3]YANG D X,LIU Y G,FANG M H,et al.Study on the slag corrosion resistance of unfired Al2O3-SiC/β-Sialon/Ti(C,N)-C refractories[J].Ceram Int,2014,40(1):1593-1598.
[4]LI X,LI Y,CHEN L,et al.Matrix structure evolution and thermo-mechanical properties of carbon fiber-reinforced Al2O3-SiC-Ccastable composites[J].Mater Res Bull,2015,61:201-206.
[5]GOGTAS C,LOPEZ H F,SOBOLEV K.Role of cement content on the properties of self-flowing Al2O3 refractory castables[J].J Eur Ceram Soc,2014,34(5):1365-1373.
[6]LEE W E,MOORE R E.Evolution of in situ Refractories in the 20th Century[J].J Am Ceram Soc,1998,29(36):1385-1410.
[7]BRAULIOL M A L,MORBIOLI G G,BITTENCOURT L R M,et al.Novel features of nanoscaled particles addition to alumina-magnesia refractory castables[J].J Am Ceram Soc,2010,93(9):2606-2610.
[8]ZHANG S,LEE W E.Carbon containing castables:current status and future prospects[J].British Ceram Transact,2002,101(1):1-8.
[9]LEE W E,ZHANG S.Melt corrosion of oxide and oxide-carbon refractories[J].Int Mater Rev,1999,44(3):77-104.
[10]WEI G,ZHU B,LI X,et al.Microstructure and mechanical properties of low-carbon Mg O-C refractories bonded by an Fe nanosheetmodified phenol resin[J].Ceram Inter,2015,41(1):1553-1566.
[11]HAMAZAKI Y,KANESHIGE T,SUMIMURA H,et al.The effect of spinel addition on Al2O3-SiC-C castables[J].Shinagawa Tech Rep,1998,41:15-24.
[12]毕玉保,王慧芳,赵万国,等.含碳浇注料用鳞片石墨的表面改性技术综述[J].材料导报,2017,31(15):108-114.BI Yubao,WANG Huifang,ZHAO Wanguo,et al.Mater Rev(in Chinese),2017,31(15):108-114.
[13]朱伯铨,管红梅,刘文超.以表面活性剂改善水对鳞片石墨的润湿性研究[J].武汉冶金科技大学学报:自然科学版,1999,22(3):242-244.ZHU Boquan,GUAN Hongmei,LIU Wenchao.J Wuhan Yejin Univ Sci Tech:Nat Sci Ed(in Chinese),1999,22(3):242-244.
[14]宋林喜,王林俊,张积礼.石墨微粒对MgO-MgO·Al2O3-C浇注料性能的影响[J].耐火材料,2004,38(2):79-81.SONG Linxi,WANG Linjun,ZHANG Jili.Refractories(in Chinese),2004,38(2):79-81.
[15]赵臣瑞,张三华,王冠,等.造粒石墨加入量对Al2O3-SiC-C质浇注料性能的影响[J].耐火材料,2014,48(1):54-57.ZHAO Chenrui,ZHANG Sanhua,WANG Guan,et al.Refectories(in Chinese),2014,48(1):54-57.
[16]DING J,DENG C J,ZHANG X J,et al.Synthesis of titanium carbide coating on surface of graphite by molten salt media[J].J Funct Mater,2014,45(3):03066-03069+03074.
[17]DUTTA S,DAS P,DAS A,et al.Significant improvement of refractoriness of Al2O3-C castables containing calcium aluminate nano-coatings on graphite[J].Ceram Int,2014,40(3):4407-4414.
[18]肖国庆,石佳佳,丁冬海.含碳铝酸钙粉体的燃烧合成及其微观表征[J].硅酸盐学报,2018(6):1-8.XIAO Guoqing,SHI Jiajia,DING Donghai.J Chin Ceram Soc,2018(6):1-8.
[19]YOSHIMATSU H,FUJIWARA S,KONISHI R,et al.Wettability by water and oxidation resistance of alumina-coated graphite powder[J].JCeram Soc Jpn,1995,103(9):929-934.
[20]DONNET J B,VOET A.Carbon black:physics,chemistry,and elastomer reinforcement[J].J Colloid Interf Sci,1977,62(1):195-196.
[21]高礼旋.炭黑的表面改性与包覆[D].广州:华南理工大学,2010.GAO Lixuan,Surface modification and encapsulation of carbon black(in Chinese,dissertation).Guangzhou:South China of Technology,2010.
[22]WANG Y,Li X,ZHU B,et al.Microstructure evolution during the heating process and its effect on the elastic properties of CAC-bonded alumina castables[J].Ceram Int,2016,42(9):11355-11362.
[23]DUTTA S,DAS P,DAS A,et al.Physical characteristics of alumina-carbon refractory castables containing calcium aluminate coated graphites[J].Inter Refract Man,2013,62(4):294-298.
[24]ZHANG J,JIA Q,YAN S,et al,Microstructure and properties of hydratable alumina bonded bauxite-andalusite based castables[J],Ceram Int,2016,42(1):310-316.