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层状苯膦酸-磷酸锆的合成与磺化研究 总被引:2,自引:0,他引:2
研究了制备苯膦酸-磷酸锆Zr(PO4H)2-n(PO3Ph)n的主要影响因素。在F-/Zr4+=12和H3PO4/Zr4+=20条件下,通过改变苯膦酸用量获得了n=0~2的系列单一晶相层状苯膦酸-磷酸锆,其热稳定性达400℃以上。苯膦酸-磷酸锆的磺化试验表明层间苯环可被完全磺化,磺化产物Zr(PO4H)2-n(PO3PhSO3H)n具有丰富的酸性位,其热稳定性亦可达到300℃以上。 相似文献
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磺化甲苯膦酸锆的制备及催化反应研究 总被引:4,自引:0,他引:4
首次制得磺化甲苯膦酸锆(ZSTP),用X-衍射、热重量分析、红外光谱、元素分析等进行了表征。并以磺化甲苯膦酸锆为固体酸催化剂对酯化、缩醛、缩酮、醇脱水成醚、成烯等有机反应进行了研究。ZSTP催化的反应收率高,操作简便,后处理容易,催化剂可以重复使用和再生。 相似文献
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含膦,氮配体的混合膦酸锆—钯催化剂的研制 总被引:6,自引:3,他引:6
用氯化二苯基膦为膦化试剂,首次对多乙烯多胺乙基膦酸-磷酸氢锆Zr(HPO4)1.35(O2PCH2CH2(NHCH2CH2)mNH2)0.65·H2O(ZP-PEPAEPA,n=0,1,2,3,4)载体表面进行二苯基膦化,合成了一类含膦氮配体的新型混合膦酸锆载体及负载钯催化剂。研究了有机膦酸侧链不同链长和Ph2PCl用量对配体载体制备的影响,并用IR,TG,DTG,DTA对这类载体及催化剂进行表征 相似文献
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于220℃水热晶化下制备了高结晶度的γ-ZrP,合成了3种γ-苄基膦酸-磷酸锆层状化合物Zr(PO4).(H2PO4)0.15(C6H5CH2PO3H)0.85·0.4H2O(1,d=1.86nm),Zr(PO4)(H2PO4)0.30(C6H5CH2PO3H)0.70·0.6H2O(2,d=1.78nm)和Zr(PO4)(H2PO4)0.50(C6H5CH2PO3H)0.50·0.7H2O(3,d=1.66nm).用X射线粉末衍射和31P固态核磁共振等手段表征其结构,并研究了其与α-苯乙胺的插层性能. 相似文献
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氨基酸桥联新型手性锌双卟啉配合物的合成与表征 总被引:5,自引:2,他引:5
生命系统中的金属卟啉生物大分子在卟啉的Soret带均表现出诱导圆二色性(InducedFig.1Structureofaminoacidbridgedzincpor┐phyrindimerO,O┐C2┐AA┐C2┐(TPP)2Zn2R=Bn,AA=P... 相似文献
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三苯基锗炔基膦酸酯的合成和表征 总被引:3,自引:0,他引:3
0IntroductionInrecentyears,thechemistryoforganogermaniumcompoundswasextensivelystudiedbecauseoftheirbiologicalactivity犤1,2犦.Organotinderivativesofoxyandthiophosphorusacidarewell-known犤3~5犦.Inourearlywork,theorganotinderivativesofalkynyloralkenylphosphateweresynthesizedandtheirstructuresandbiologicalactivitieswerealsostudied犤6~8犦.Sofar,tri-organogermaniumderivativesofphosphonicacidhavenotbeenreported.Inthispaper,O-bis(triphenylgermanium)alkynylphosphatesandO-trip… 相似文献
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采用壳聚糖改性棉和涤纶织物,通过织物表面的壳聚糖原位吸附、还原银离子制备了纳米银抗菌织物.用场发射扫描电子显微镜(SEM)、X射线能谱(EDA)、X射线粉末衍射仪(XRD)和反射光谱等对纳米银织物进行了表征,研究了银离子浓度和壳聚糖浓度对纳米银织物的影响,并检测了纳米银织物的抗菌性能.结果表明,在无需任何还原剂的条件下,壳聚糖改性的棉和涤纶织物表面可以均匀地形成银纳米粒子,晶粒大小为5~10 nm,所制备的纳米银织物均具有优异的抗菌性能. 相似文献
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采用间歇式鼓泡碳化法,以油酸为添加剂,通过对实验条件的控制,原位制备了由小立方体晶粒连接而成的链状纳米碳酸钙,粒子的长径比约为6∶1,分散性良好、白度高、吸油值低,并对其碳化反应机理进行了初步探讨。同时,通过电子透射电镜、X射线衍射、傅里叶红外光谱、白度和吸油值等测试手段对产物的结构和性能进行了表征。 相似文献
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GU Jin-ying HE Wan-ping SHI Xian-fa JI Liang-nian 《高等学校化学研究》2008,24(1):106-109
Three novel types of chiral calixarene derivatives 5, 8, and 10 were designed and synthesized by introducing chiral units to parent calixarenes. Their chiralities were confirmed by rotational analysis. Chiral recognition properties of these host compounds towards L- and D-threonine were studied by UV-Vis spectroscopy. The results indicated that calixarene derivatives 5 and 8 exhibited good chiral recognition capabilities toward L- or D-threonine. Although calixarene derivative 10 had no evident chiral recognition ability, the supramolecules of calixarene derivative 10 with L- or D-threonine showed a hypochromic effect or hyperchromic effect respectively. Therefore, calixarene derivative 10 might serve as a good chiral UV-indicator. 相似文献
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WANG Jianmin CAO Feng DENG Ruiping HUANG Lijian LI Song CAI Jiajia L Xin QIN Gaowu 《高等学校化学研究》2016,32(3):338-342
The evolution of morphology and heterostructure of BiOCl was investigated during an in situ oxidation reaction. Morphology and structure transformation of regular 2D nanoflake, 0D nanosphere or 3D nanoflower was achieved by adjusting the ratio of reagent concentration or reaction temperature, respectively. The enhanced photocatalytic degradation ability and the photocurrent intensity of BiOCl nanomaterials may be attributed to the improved degree of crystallinity and the formation of Bi/BiOCl heterostructure. The photocurrent density of Schottky battery was increased due to enhancing the optical pathway and assisting during charge separation. Crystallinity also contributed to the improvement of the photoelectric conversion efficiency and reduction of the recombination rate of photogenerated electron-hole pairs. 相似文献
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HU Jin ZHANG Han-Hui CAO Yan-Ning ZHANG Chun-Gang ZHANG Shuai CHEN Yi-Ping SUN Rui-Qing 《结构化学》2009,28(8):939-946
Two novel transition metal phosphonate compounds, [Co(H2BDPP)(phen)]n 1 (BDPP = p-O3PCH2(C6H4)CH2PO3, phen = 1,10-phenanthroline) and [Pb3(BCP)2]n 2 (BCP = OOC(C6H4)CH2PO3), have been synthesized and structurally determined by X-ray single-crystal diffraction. Compound 1 crystallizes in the monoclinic system, space group C2/c with a = 21.169(4), b = 12.001(2), c = 7.6211(15)A, β = 98.03(3)°, V= 1917.2(6)A^3, C20H18N2O6P2Co, Mr = 505.22, Z = 8, De= 1.737 g/cm^3, p = 1.107 mm^-1, F(000) = 1020, the final R= 0.0450 and wR = 0.1306 for 2072 observed reflections (I 〉 2σ(I). Compound 2 crystallizes in the monoclinic system, space group C2/c with a = 4.7167(9), b = 18.753(2), c = 22.781(3)A, β = 91.07(3)°, V= 2014.7(14)A^, C8H6O5PPb1.5, Mr = 523.88, Z = 8, Dc = 3.454 g/cm^3, p = 25.222 mm^-1, F(000) = 1856, the final R = 0.0441 and wR = 0.1906 for 2259 observed reflections (I 〉 2σ(I). In compound 1, the 1D chain running along the c axis is bridged by four ligands (trans- HO3PCH2C6H4CH2PO3H) in four different directions to extend the structure into a three- dimensional network. In compound 2, the Pb(II) displays 4- and 5-coordination modes. There is a one-dimensional P-O-Pb band along the a axis formed by PO3 groups and Pb(II) cations. These bands are joined by μ2-O of -COO to yield two-dimensional inorganic P-O-Pb layers which are pillared by the OOCC6HaCH2PO3 ligands to form a three-dimensional network. Moreover, compound 2 displays a strong emission band attributed to the ligand-centered (LC) transition. 相似文献
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NENU-n系列多酸基金属有机框架杂化物(POM@MOFs)是将一系列性能优异的Keggin型杂多酸封装到Cu3(BTC)2框架中形成的, 在催化和质子传导等领域展示出优异的性能. 本文在前期工作的基础上发展了一种在铜箔上原位合成POM@MOFs的新方法, 即向反应液中通入氧气, 利用酸性条件下氧气能将Cu0氧化为Cu2+的特性为金属有机框架的生长提供铜离子源, 使氧化能力较弱的Keggin型钨系杂多酸也可在铜基底上原位合成纯相NENU-n系列杂化物. 该方法可在室温条件下进行, 简便、 快速且原子经济性高. 同时发现在不添加任何调节剂的条件下, 利用该方法能生成形貌可控的POM@MOFs, 其形貌依赖于杂多酸阴离子所带的电荷. 电荷高的杂多阴离子可以得到立方体形貌, 而电荷低的杂多阴离子得到八面体形貌. 利用合成的材料对芥子气模拟物2-氯乙基乙基硫醚(CEES)的催化氧化反应进行了研究, 结果表明暴露活性位点更多的立方体形貌的NENU-40[K5BW12O40/Cu3(BTC)2]展现出更优异的催化活性, 10 min内即可将2-氯乙基乙基硫醚完全转化为无毒的亚砜. 相似文献
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合成了七种见文献报道的硫酸镧与氨基酸的配合物,通过化学分析,元素分析,红外光谱和热分析等,确定了所得配合物的组成为La2(AA)n(SO4)3.xH2O(AA=氨基酸;n=4,4,6;x=4,6,8),并对它们的荧光光谱等进行了研究。 相似文献
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以1,6-己二胺为模板剂的层状磷酸锆晶体的合成与表征 总被引:1,自引:0,他引:1
采用水热法合成了以1,6-己二胺(HDA)为模板剂的层状磷酸锆晶体0.5·1.5H2O,并用单晶及粉末XRD,IR和TG-DTA等对其结构和性质进行了表征. 该晶体是由磷酸锆无机层、有机胺以及水分子三部分构成的层状结构,层间距约为1.77 nm,无机层结构为γ-型. 位于有机胺两端的氮与无机层表面部分羟基的氧以氢键连接,水分子占据磷酸锆层间的两种位置. 单晶结构模拟得到的XRD谱与从粉末样品采集的XRD谱基本吻合. 此晶体在180 ℃下脱去水分子,在220 ℃下加热3 h其结构未发生明显变化; 有机胺模板剂在250 ℃下开始分解. 相似文献