烧结温度对氧化铝陶瓷膜支撑体性能的影响
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摘要
实验以α-Al_2O_3为骨料,TiO_2-MnO_2-MgO为复相烧结助剂,采用挤压成型法和固态粒子烧结法制备Al_2O_3陶瓷膜支撑体,并探究烧结温度对陶瓷膜支撑体性能的影响。通过压汞法、自制纯水通量测定装置、三点弯曲法、质量损失法、X-射线衍射(XRD)、扫描电镜(SEM)等方法对α-Al_2O_3陶瓷支撑体的孔隙率、纯水通量、抗折强度、酸碱腐蚀率、晶相变化以及表面形貌等微观结构进行分析表征。研究结果表明:TiO_2-MnO_2-MgO能显著降低α-Al_2O_3陶瓷支撑体的烧结温度,烧结温度低于800℃,无法提供足够的激活能,支撑体没有新相生成;超过1 300℃时,支撑体纯水通量随着烧结温度升高而急剧下降。当烧结温度为1 300℃时,制得的支撑体性能良好,孔隙率达到了44.84%、抗折强度为80.21 MPa、纯水通量为8 979.37 L/(m~2·h·MPa)、酸/碱腐蚀质量损失率为0.87%/1.09%。
Tubular porous alumina ceramic support with α-Al_2O_3 as aggregate,TiO_2-MnO_2-MgO as multiphase sintering agent was prepared by extrusion-forming and solid sintering method.The effect of sintering temperature on the properties of ceramic membrane support was mainly studied.The porosity,pure water flux,flexural strength,acid and alkali corrosion,crystal phases and surface morphology of α-Al_2O_3 ceramic support were analyzed by testing methods such as Mercury intrusion method,self-made pure water flux measurement device,Three-point bending method,Mass loss method,X-ray diffraction(XRD) and Scanning electron microscope(SEM).The results show that TiO_2-MnO_2-MgO can reduce the sintering temperature of the α-Al_2O_3 ceramic support significantly.When the sintering temperature is below 800 ℃,the activation energy can not be provided enough and without any new phase in the support.When the sintering temperature is above 1 300 ℃,the pure water flux of the support decreases sharply with the increase of sintering temperature.When the sintering temperature is 1 300 ℃,the prepared support has a good performance with a porosity of 44.84%,the flexura strength is 80.21 MPa,the pure water flux is 8 979.37 L/(m~2·h·MPa),the mass loss rate of acid/alkali corrosion is only 0.87%/1.09%.
Tubular porous alumina ceramic support with α-Al_2O_3 as aggregate,TiO_2-MnO_2-MgO as multiphase sintering agent was prepared by extrusion-forming and solid sintering method.The effect of sintering temperature on the properties of ceramic membrane support was mainly studied.The porosity,pure water flux,flexural strength,acid and alkali corrosion,crystal phases and surface morphology of α-Al_2O_3 ceramic support were analyzed by testing methods such as Mercury intrusion method,self-made pure water flux measurement device,Three-point bending method,Mass loss method,X-ray diffraction(XRD) and Scanning electron microscope(SEM).The results show that TiO_2-MnO_2-MgO can reduce the sintering temperature of the α-Al_2O_3 ceramic support significantly.When the sintering temperature is below 800 ℃,the activation energy can not be provided enough and without any new phase in the support.When the sintering temperature is above 1 300 ℃,the pure water flux of the support decreases sharply with the increase of sintering temperature.When the sintering temperature is 1 300 ℃,the prepared support has a good performance with a porosity of 44.84%,the flexura strength is 80.21 MPa,the pure water flux is 8 979.37 L/(m~2·h·MPa),the mass loss rate of acid/alkali corrosion is only 0.87%/1.09%.
引文
[1]MALLADA R,MENENDEZ M.Inorganic membranes synthesis,characterization and application[M].Amsterdam:Elsevier Press,2008:217-245.
[2]NG Kok-Kwang,LIN Cheng-Fang,SRI CHANDANA P,et al.Reduced membrane fouling in novel bio-entrapped membrane reactor for treatment of food and beverage processing wastewater[J].Water Research,2011,45:4269-4278.
[3]杨柯,常启兵,王霞,等.高岭土为助烧剂制备多孔陶瓷膜支撑体[J].中国陶瓷,2012,48(9):24-26.
[4]SILVA L O,VASCONCELOS C L,NUNES H M,et al.Processing,structural characterization and performance of alumina supports used in ceramic membranes[J].Ceramics International,2012,38(3):1943-1949.
[5]郭坚,张超,徐鹏,等.氧化物多孔陶瓷制备工艺的研究进展[J].硅酸盐通报,2013,32(11):2292-2296.
[6]苏魁范,邓湘云,李建保,等.复合碳化硅陶瓷过滤膜材料的制备及表征[J].膜科学与技术,2013,33(2):18-23.
[7]陈菊红,陶杰,朱碧肖,等.多孔氧化铝陶瓷膜支撑体的制备与表征[J].过滤与分离,2014,25(1):12-16.
[8]BONEKAMP B C.Preparation of asymmetric ceramic membrane supports by dip-casting[M]//BURGGRAAF A J.Fundamentals of inorganic membrane science and technology.Amsterdam:L Cot Elsevier Press,1996:141-221.
[9]孟凡朋,樊震坤,张健,等.挤出法制备陶瓷膜支撑体工艺过程及影响因素研究进展[J].山东陶瓷,2017,40(1):3-7.
[10]陈仕俊,余阳,林晓亮,等.低温烧结制备氧化铝陶瓷膜支撑体[J].人工晶体学报,2017,46(5):826-831.
[11]范益群,漆虹,徐南平.多孔陶瓷膜制备技术研究进展[J].化工学报,2013,64(1):107-115.
[12]漆虹,刑卫红,范益群.低温烧成高纯Al2O3多孔陶瓷膜支撑体的制备[J].硅酸盐学报,2010,38(2):283-293.
[13]ZHANG Qilong,YANG Hui,ZOU Jiali,et al.Sintering and dielectric properties of Al2O3ceramics doped by Ti O2and Cu O[J].Joural of Electroceram,2007,18:225-229.
[14]朱庆鹏.多孔氧化铝陶瓷膜支撑体的制备及其性能表征[D].西安:西安工程大学,2011.
[15]李小斌,徐晓辉,周秋生.氧化铝多孔陶瓷膜支撑体制备的工艺过程和微观机制的综合评述[J].矿冶工程,2003,23(6):62-64.
[16]罗儒显,黄仲涛.固态粒子烧结法制α-Al2O3陶瓷膜管的研究(I)[J].五邑大学学报,1996,10(1):1-7.
[17]杨京生.GB/T1970-1996多孔陶瓷耐酸、碱腐蚀性能试验方法[S].北京:中国标准出版社,1996.
[18]吴振东,叶建东.添加剂对氧化铝陶瓷的烧结和显微结构的影响[J].兵器材料科学与工程,2002,25(1):68-72.
[2]NG Kok-Kwang,LIN Cheng-Fang,SRI CHANDANA P,et al.Reduced membrane fouling in novel bio-entrapped membrane reactor for treatment of food and beverage processing wastewater[J].Water Research,2011,45:4269-4278.
[3]杨柯,常启兵,王霞,等.高岭土为助烧剂制备多孔陶瓷膜支撑体[J].中国陶瓷,2012,48(9):24-26.
[4]SILVA L O,VASCONCELOS C L,NUNES H M,et al.Processing,structural characterization and performance of alumina supports used in ceramic membranes[J].Ceramics International,2012,38(3):1943-1949.
[5]郭坚,张超,徐鹏,等.氧化物多孔陶瓷制备工艺的研究进展[J].硅酸盐通报,2013,32(11):2292-2296.
[6]苏魁范,邓湘云,李建保,等.复合碳化硅陶瓷过滤膜材料的制备及表征[J].膜科学与技术,2013,33(2):18-23.
[7]陈菊红,陶杰,朱碧肖,等.多孔氧化铝陶瓷膜支撑体的制备与表征[J].过滤与分离,2014,25(1):12-16.
[8]BONEKAMP B C.Preparation of asymmetric ceramic membrane supports by dip-casting[M]//BURGGRAAF A J.Fundamentals of inorganic membrane science and technology.Amsterdam:L Cot Elsevier Press,1996:141-221.
[9]孟凡朋,樊震坤,张健,等.挤出法制备陶瓷膜支撑体工艺过程及影响因素研究进展[J].山东陶瓷,2017,40(1):3-7.
[10]陈仕俊,余阳,林晓亮,等.低温烧结制备氧化铝陶瓷膜支撑体[J].人工晶体学报,2017,46(5):826-831.
[11]范益群,漆虹,徐南平.多孔陶瓷膜制备技术研究进展[J].化工学报,2013,64(1):107-115.
[12]漆虹,刑卫红,范益群.低温烧成高纯Al2O3多孔陶瓷膜支撑体的制备[J].硅酸盐学报,2010,38(2):283-293.
[13]ZHANG Qilong,YANG Hui,ZOU Jiali,et al.Sintering and dielectric properties of Al2O3ceramics doped by Ti O2and Cu O[J].Joural of Electroceram,2007,18:225-229.
[14]朱庆鹏.多孔氧化铝陶瓷膜支撑体的制备及其性能表征[D].西安:西安工程大学,2011.
[15]李小斌,徐晓辉,周秋生.氧化铝多孔陶瓷膜支撑体制备的工艺过程和微观机制的综合评述[J].矿冶工程,2003,23(6):62-64.
[16]罗儒显,黄仲涛.固态粒子烧结法制α-Al2O3陶瓷膜管的研究(I)[J].五邑大学学报,1996,10(1):1-7.
[17]杨京生.GB/T1970-1996多孔陶瓷耐酸、碱腐蚀性能试验方法[S].北京:中国标准出版社,1996.
[18]吴振东,叶建东.添加剂对氧化铝陶瓷的烧结和显微结构的影响[J].兵器材料科学与工程,2002,25(1):68-72.