摘要
采用并流滴加溶剂热法,研究了合成温度对MOF-5材料热稳定性的影响规律,并确定了最佳合成工艺条件.XRD分析表明,合成的MOF-5材料纯度高、结晶性好;FTIR分析表明—C==O伸缩振动峰与对苯二甲酸相比发生了明显的红移,对苯二甲酸完全去质子化为MOF-5材料合成提供了必要条件;SEM分析表明其形貌在140℃下为片状,160℃下为棱柱状;结合TGA分析表明,在一定温度范围内,随着合成温度的升高,其形貌由片状向棱柱状转变,且热稳定性也逐渐提高,最高热分解温度为491.95℃.
The rule of influence of synthetic temperature on thermal stability of material MOF-5 was investigated with parallel drop solvothermal method and the optimum synthetic process conditions were determined.The XRD analysis of the synthesized material MOF-5 showed that the synthetic would be of high purity and good crystallinity.The FTIR analysis showed that the—C==O stretching vibration peak would have a remarkable red shift compared with the case of terephthalic acid,which would be completely deprotonated and provide the necessary conditions for material synthesis of MOF-5.The SEM analysis showed that its morphology would be lamellar at 140 ℃ and prismatic at 160 ℃.TGA analysis showed that in a certain temperature range,with the increase of synthesising temperature,the morphology would changes from flaky to prismy,and its thermal stability would also increase gradually,its maximum thermal decomposition temperature being 491 ℃.
引文
[1]CHANDAN D,TANAY K,BISHNU P B,et al.Crystalline metal-organic frameworks(MOFs):synthesis,structure and function[J].Crystal Engineering,2014,70(1):3-10.
[2]王丹,方师豪,谷小丹,等.金属有机骨架材料MOF-5的制备及其在染料废水治理中的应用研究[J].辽宁化工,2015,44(7):793-795.
[3]EDDAOUDI M,KIM J,ROSI N,et al.Systematic design of pore size and functionality in isoreticular MOFs and their application in methane storage[J].Science,2002,295(5554):469-472.
[4]张毅,杨先贵,王庆印,等.硝基修饰MOF-5材料的制备及催化氨基甲酸酯热分解[J].高等学校化学学报,2014,35(3):613-618.
[5]LUN D J,TELFER S G A.General Thermolabile Protecting group strategy for organocatalytic metal-organic frameworks[J].Am Chem Soc,2011,133(15):5806-5809.
[6]CHATTI R,THOTE JAYASHRI A,KUMAR V,et al.Amine loaded zeolites for carbon dioxide capture:amine loading and adsorption studies[J].Microporous and Mesoporous Materials,2009,121(3):84-89.
[7]WANG G,FAN Y,XU J N,et al.A porous lanthanide metalorganic framework with luminescent property,nitrogen gas adsorption and high thermal stability[J].Inorg Chem Comm,2010,13(1):95-97.
[8]WANG Jifeng,SHI Bingbing,LI Gang.Preparations and characterizations of two MOFs constructed with hydroxylphenyl imidazole dicarboxylate[J].Chinese Chemical Letters,2015,26(4):1059-1064.
[9]钟玮,吴孙涛,简思平.烧结金属有机骨架材料制备多孔材料及其应用[J].广东化工,2014,41(273):91-92.
[10]Sebastian Zuluaga,Erika M A Fuentes-Fernandaz,Kui Tan,et al.Understanding and controlling water stability of MOF-74[J].J Mater Chem A,2016,4:5176-5183.
[11]PARK K S,NI Z,C OTA P,et al.Exceptional chemical and thermal stability of zeolitic imidazolate frameworks[J].Proc Natl Acad Sci,2006,103(27):10186-10191.
[12]KANG I J,KHAN N A,HAQUE E,et al.Chemical and thermal stability of isotypic metal-organic frameworks:effect of metal ions[J].Chem Eur J,2011,17(23):6437-6442.
[13]WANG Pengfei,WU Xiaoshuo,WEI Bo,et al.Syntheses,crystal structures,thermal stabilities of nickel(Ⅱ)coordination polymers constructed from the substitutional benzenedicarboxylic acid and auxiliary N-Donor ligands[J].Chinese journal of inorganic chemistry,2014,30(7):1511-1517.
[14]CAVKA J H,JAKOBSEN S,OLSBYE U,et al.A new airconium inorganic building brick forming metal organic frameworks with exceptional stability[J].J Am Chem Soc,2008,130(42):13850-13851.
[15]张晓东,李红欣,侯扶林,等.金属有机骨架材料MOF-5的制备及其吸附CO2性能研究[J].功能材料,2016,47(8):8178-8181.
[16]WANG Lei,WANG Cong,SUN Ying,et al.Large negative thermal expansion provided by metal-organic framework MOF-5:A first-principles study[J].Materials Chemistry and Physics,2016,175(1):138-145.
[17]Samir Alghool,Carla Slebodnick.One dimensional structure of Zn(Ⅱ)metal organic framework(MOF)assembled rapidly at room temperature:structural,thermal study,and luminescent properties[J].Inorg Organomet Polym,2014,24(3):644-651.
[18]ISAEVA V I,BELYAEVA E V,FITCH A N,et al.Synthesis and structural characterization of a series of novel Zn(Ⅱ)-based MOFs with pyridine-2,5-dicarboxylate linkers[J].Crystal Growth Design,2013,13(3):5305-5315.
[19]SUN Yinxia,SUN Weiyin.Influence of temperature on metalorganic frameworks[J].Chinese Chemical Letters,2014,25(6):823-828.
[20]MCKINSTRY C,CATHCART R J,CUSSEN E J,et al.Scalable continuous solvothermal synthesis of metal organic framework(MOF-5)crystals[J].Chemical Engineering Journal,2016,285(1):718-725.
[21]YANG Huimin,LIU Xian,SONG Xiuli,et al.In situ electrochemical synthesis of MOF-5and its application in improving photocatalytic activity of BiOBr[J].Trans Nonferrous Met Soc China,2015,25(12):3987-3994.
[22]DURETTE D,BNARD P,ZACHARIA R,et al.Investigation of the hydrogen adsorbed density inside the pores of MOF-5from path integral grand canonical Monte Carlo at supercritical and subcritical temperature[J].Sci Bull,2016,61(8):594-600.
[23]Nazmul Abedin Khan,Sung Hwa Jhung.Synthesis of metalorganic frameworks(MOFs)with microwave or ultrasound:Rapid reaction,phase-selectivity,and size reduction[J].Coordination Chemistry Reviews,2015,285(15):11-23.
[24]ZHOU You,LIU Changjun.Amorphization of metal-organic framework MOF-5by electrical discharge[J].Plasma Chem Plasma Process,2011,31(3):499-506.
[25]SEGAKWENG T,MUSYOKA N M,REN J,et al.Comparison of MOF-5and Cr-MOF derived carbons for hydrogen storage application[J].Res Chem Intermed,2016,42(5):4951-4961.
[26]姜宁,邓志勇,刘绍英,等.常压合成MOF-5及其吸附CO2的研究[J].应用化工,2016,45(11):2013-2016.
[27]袁长福,刘晋,韩鹏飞,等.MOF-5对PEO基电解质导锂及界面稳定性能的改善[J].中南大学学报(自然科学版),2015,46(4):1189-1196.
[28]HAN Pengfei,YUAN Changfu,XU Junyi,et al.Synthetic control method for crystallite size of MOF-5[J].Chem Res Chin Univ,2014,30(3):356-361.
[29]MING Yang,PUREWAL J,LIU Dong’an,et al.Thermophysical properties of MOF-5powders[J].Microporous and Mesoporous Materials,2014,185(1):235-244.
[30]Srinivas Gadipelli,GUO Zhengxiao.Postsynthesis annealing of MOF-5remarkably enhances the framework structural stability and CO2 uptake[J].Chemistry of Materials,2014,26(22):6333-6338.