膦酸锆、杂化磷酸锆的合成、表征插层及催化性能研究
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摘要
膦酸锆、杂化磷酸锆的合成、表征、插层及催化研究对于主-客体超分子化学、多功能材料的性质、制备、应用和开发具有重要意义。本文通过类Mannich方法合成了10种α-氨基膦酸衍生物,进行了元素分析、红外光谱(FTIR)、核磁共振氢谱(1H NMR)和核磁共振磷谱(31P NMR)等表征,详细讨论了它们的结构。
本文合成了层状甲基、乙基、丙基、丁基、庚基、癸基-N,N-双甲基膦酸锆主体及相应的6种苯胺插层化合物,并进行了元素分析、电感偶合等离子发射光谱(ICP)、X射线粉末衍射(XRD)、红外光谱(FTIR)、激光拉曼光谱(Raman Spectra)、扫描电镜(SEM)、热重分析(TG-DSC)等表征。结果表明6种膦酸锆组成:Zr(O3PCH2)2N(CH2)nCH3·xH2O (n=0,1,2,3,6,9),层间距:1.046～1.962 nm,其结构;带有机侧链的双膦酸连在主体的同一层板上。苯胺插层化合物组成:Zr(O3PCH2)2N(CH2)nCH3·xC6H5NH2·yH2O,层间距:1.097～2.526 nm,苯胺以单分子层排列于主体层间。苯胺聚合反应结果表明聚苯胺并没有包夹在主体层间,而是分散在主体微粒之间。
本文合成了x=1.0的层状晶态和无定形脯氨酸-N-甲基膦(磷)酸锆(分别记为:α-ZLPMPAx=1和ZLPMPAx=1),并进行了相应表征。α-ZLPMPAx=1的组成:Zr(O3PG)(HPO4)·H2O,层间距:1.520 nm,理想结构模型:有机基团与无机基团尽可能均匀地交错排布。通过振荡法、回流法和微波法研究了丁胺(BA)、庚胺(HA)、癸胺(DA)、精氨酸(Arg)、赖氨酸(Lys)、组氨酸(His)等碱性客体分子与α-ZLPMPAx=1主体的插层反应,每个α-ZLPMPAx=1主体分子分别嵌入:0.43 BA、0.34 HA、0.33 DA、0.20 Arg、0.54 Lys和0.39 His。插层化合物α-ZLPMPAx=1-BA、α-ZLPMPAx=1-HA、α-ZLPMPAx=1-DA成功地吸附了酚。
本文合成了4种层状晶态、无定形甘氨酸-N,N-双甲基膦(磷)酸锆(分别记为:α-ZGMDPAx=0.66、α-ZGMDPAx=2、ZGMDPAx=0.66、ZGMDPAx=2),并进行了相应表征。α-ZGMDPAx=0.66、α-ZGMDPAx=2的组成分别为: Zr[(O3PCH2)2NCH2COOH]0.33 (HPO4)1.34·0.70 H2O和Zr[(O3PCH2)2NCH2COOH]·H2O,层间距分别为:1.542和1.271 nm。考察了烷基单胺(甲胺(MA)、乙胺(EA)、丙胺(PA)、BA、HA、DA)、烷基多胺(乙二胺(1E2A)、二乙基三胺(2E3A)、三乙基四胺(3E4A)、四乙基五胺(4E5A)、1,3-丙二胺( PDA))和六氢吡啶(HHP)等客体分子与α-ZGMDPAx=0.66、α-ZGMDPAx=2主体的插层反应。烷基单胺、杂环化合物以双分子层排列于α-ZGMDPAx=0.66主体层间,烷基多胺在α-ZGMDPAx=0.66、α-ZGMDPAx=2主体中产生了多种排列方式。
本文以无定形ZLPMPAx=1、ZGMDPAx=0.66、ZGMDPAx=2为载体制备了固体碱,固体碱强度H-:9.3～15.0,在微波辐射、无溶剂或加热条件下,催化芳香醛与活泼亚甲基化合物的Knoevenagel反应产率:76.4～91.1 %,能重复使用4次以上,是一类环境友好催化剂。ZGMDPAx=0.66固载钯配合物催化Suzuki反应的取代联苯产率:81.4 %。
本文合成了6种不同x值的层状晶态和无定形苄基-N,N-双甲基膦(磷)酸锆(分别记为:α-ZBMDPA、ZBMDPA),并进行了相应表征。α-ZBMDPAx=1.0的组成:Zr[C6H5CH2N(CH2PO3)2]0.5(HPO4)·2.1 H2O,层间距:2.034 nm,其理想结构:层间苯环与苯环相对。详细研究了α-ZBMDPAx=1.0的插层反应性能,成功地将客体分子:烷基单胺(MA、二甲胺(DMA)、三甲胺(TMA)、EA、二乙胺(DEA)、三乙胺(TEA)、PA、BA、二丁胺(DBA)、三丁胺(TBA)、HA、DA)、烷基多胺(1E2A、2E3A、3E4A、4E5A、PDA)、杂环化合物(四氢吡咯(TPR)、HHP、吗啉(ML)、哌嗪(PH))嵌入层状化合物α-ZBMDPAx=1.0层间,烷基单胺、杂环化合物在α-ZBMDPAx=1.0主体层间单分子层排列并与主体层板倾斜成一定角度,烷基多胺也有多种排列方式。插层化合物α-ZBMDPAx=1.0-BA\α-ZBMDPAx=1.0HA、α-ZBMDPAx=1.0-DA成功地吸附了酚,α-ZBMDPAx=1.0-3E4A、α-ZBMDPAx=1.04E5A吸附了甲醛。
本文合成了无定形ZBMDPA载体固载多胺(1E2A、2E3A、3E4A、4E5A)配体及4种钯配合物,进行了FTIR、原子吸收光谱(AAS)、X射线光电子能谱(XPS)、XRD等表征,苄基-N,N-双甲基膦(磷)酸锆多胺配体固载钯配合物催化卤代芳烃与芳基硼酸的Suzuki反应,结果表明碘代芳烃偶联反应产率:92.1 %,催化剂与产物分离容易,催化剂能重复使用5次以上,而对溴代芳烃和氯代芳烃催化活性较低。本文通过微波辐射、超声波震荡、回流法等研究了His、Arg、Lys与α-Zr(HPO4)2·H2O(α-ZrP)的超分子插层组装,这些客体以单分子层排列在α-ZrP主体层间,每个α-ZrP分子分别嵌入:0.50 His、0.13 Arg和0.84 Lys。插层化合物α-ZrP-His对水相中丙酮与4-硝基苯甲醛Aldol反应具有一定的催化活性和一定的重复使用性,是一类值得进一步研究的多相催化材料。
It is very important to study synthesis, characterization, intercalation and catalysis of zirconium phosphonates and hybrid zirconium phosphates for host-guest supermolecule chemistry, property, preparation, application and development of multifunctional materials.
In this paper, 10 kinds ofα-aminomethylphosphonic acid derivitives were synthesized by the Mannich-type reaction. The property and structure ofα-aminomethylphosphonic acid derivitives were characterized and discussed by elemental analysis, Fourier Transform Infrared Transmission-absorption Spectra (FTIR), Nuclear Magnetic Resonance (1H NMR and 31P NMR) in detail.
12 kinds of layered zirconium dimethylphosphonates and aniline intercalation compounds were synthesized and characterized by elemental analysis, Inductive Coupled Plasma Emission Spectrum (ICP), X-ray Powder Diffraction (XRD), FTIR, Laser Raman Spectra (Raman Spectra), Scanning Electron Microscope (SEM), Thermogravimetry and Differential Scanning Calorimetry (TG-DSC). The results demonstrated that the compositions of zirconium phosphonates were Zr(O3PCH2)2N(CH2)nCH3·xH2O (n=0, 1, 2, 3, 6, 9) with the interlayer distances of 1.046 nm to 1.962 nm, two dimethylphosphonates might bind to the same layer. The compositions of aniline intercalation compounds were Zr(O3PCH2)2N(CH2)nCH3·xC6H5NH2·yH2O with the interlayer distances of 1.097 nm to 2.526 nm, and anilines arranged as monomolecular layers in the gallery of these hosts. The polymerization of aniline showed that polyaniline was not inserted between the layers of host, but diffused in the particles of host.
2 kinds of layered crystalline and amorphous zirconium proline-N-methylphosphonate-phosphates (α-ZLPMPAx=1 and ZLPMPAx=1) were synthesized and characterized by the above methods, the results indicated that the composition ofα-ZLPMPAx=1 was Zr(O3PG)(HPO4)·H2O with the interlayer distance of 1.520 nm, the N-methylproline groups and P-OH arranged alternatively. The intercalations of butylamine (BA), heptylamine (HA), decylamine (DA), arginine (Arg), lysine (Lys) and histidine (His) withα-ZLPMPAx=1 host had been studied by shaking, refluencing and microwave irradiation, 0.43 BA, 0.34 HA, 0.33 DA, 0.20 Arg, 0.54 Lys and 0.39 His inserted into in the gallery of one moleculeα-ZLPMPAx=1 host, respectively. The intercalation compoundsα-ZLPMPAx=1-BA,α-ZLPMPAx=1-HA andα-ZLPMPAx=1-DA had successfully adsorbed phenol, 4-chlorophenol and 2,4-dichlorophenol.
4 kinds of layered crystalline and amorphous zirconium glycine-N,N-dimethylphosphonate-phosphate (α-ZGMDPAx=0.66,α-ZGMDPAx=2, ZGMDPAx=0.66 and ZGMDPAx=2) had been prepared and characterized by the above methods. The compositions ofα-ZGMDPAx=0.66 andα-ZGMDPAx=2 were Zr[(O3PCH2)2NCH2COOH]0.33 (HPO4)1.34·0.70 H2O and Zr[(O3PCH2)2NCH2COOH]·H2O, the interlayer distances of them were 1.542 nm and 1.271 nm, respectively. It was found that the intercalations of alkylmonoamines (methylamine (MA), ethylamine (EA), propylamine (PA), BA, HA, DA), polyamines (ethylenediamine (1E2A), diethylenetriamine (2E3A), triethylenetetramine (3E4A), tetrathylenepentamine (4E5A), 1,3-propyldiamine (PDA)), hexahydropyridine (HHP) withα-ZGMDPAx=0.66 andα-ZGMDPAx=2 hosts, alkylmonoamines and heterocyclic compounds arranged as bimolecular layers in the gallery ofα-ZGMDPAx=0.66, polyamines formed multi-array in the gallery ofα-ZGMDPAx=0.66 andα-ZGMDPAx=2.
The solid bases with H-=9.3 to 15.0 were prepared by the amorphous supports ZLPMPAx=1, ZGMDPAx=0.66 and ZGMDPAx=2. The Knoevenagel condensations of aromatic aldehydes with active methylene compounds were catalyzed by the solid base in yield of 76.4 % to 91.1 % under microwave irradiation and solvent-free, or heating, the solid base could be reused four times. The solid base is a new type of environmentally benign catalyst. On the meanwhile the palldium complex supported on ZGMDPAx=0.66 exhibited a yield of 81.4 % for Suzuki cross-coupling reaction.
6 kinds of layered crystalline and amorphous zirconium benzyl-N,N-dimethylphosphonate-phosphates (α-ZBMDPA, ZBMDPA) were also prepared and characterized by the above methods. The composition ofα-ZBMDPAx=1.0 with the interlayer distance of 2.034 nm was Zr(HPO4)(C6H5CH2N(CH2PO3)2)0.5?2.1 H2O, and two phenyl ofα-ZBMDPAx=1.0 double layers faced to face each other. Alkylmonoamines (MA, dimethylamine (DMA), trimethylamine (TMA), EA, diethylamine (DEA), triethylamine (TEA), PA, BA, dibutylamine (DBA), tributylamine (TBA), HA, DA), polyamines (1E2A, 2E3A, 3E4A, 4E5A, PDA), heterocyclic compounds (pyrrolidine (TPR), HHP, morpholine (ML), piperazine(PH)) had successfully inserted into the gallery ofα-ZBMDPAx=1 host, alkylmonoamines and heterocyclic compounds arranged as monomolecular layers in the gallery ofα-ZBMDPAx=1, polyamines also formed multi-array in the gallery of.α-ZBMDPAx=1. The intercalation compoundsα-ZBMDPAx=1-BA,α-ZBMDPAx=1-HA andα-ZBMDPAx=1-DA adsorbed phenol, 4-chlorophenol and 2,4-dichlorophenol,α-ZBMDPAx=1-3E4A andα-ZBMDPAx=1-4E5A adsorbed formaldehyde.
Series of pallidum complexes were prepared by introducing the ligand polyamines (1E2A, 2E3A, 3E4A and 4E5A) into the support ZBMDPA. These pallidum complexes supported on ZBMDPA polyamines were characterized by FTIR, Atomic Absorption Spectra (AAS), X-ray Photoelectron Spectra (XPS) and XRD. The pallidum complexes catalyzed Suzuki cross-coupling reaction of aryl halides with aryl boronic acids, compared with aryl bromides and aryl chloride, aryl iodide obtained better yield (92.1%), the catalyst could be easily recovered and reused more than five times.
In addition, the intercalations of His, Arg, Lys withα-Zr(HPO4)2·H2O (α-ZrP) had been studied under microwave irradiation, ultrasound and refluencing, these amino acids arranged as monomolecular layers, 0.50 His, 0.13 Arg and 0.84 Lys inserted into the gallery of one moleculeα-ZrP, respectively. The intercalation compoundα-ZrP-His catalyzed Aldol reaction of acetone with 4-nitrobenzaldehyde in proper yield and could be reused. It is necessary to researchα-ZrP-His as multiphase catalysis materials.
本文合成了层状甲基、乙基、丙基、丁基、庚基、癸基-N,N-双甲基膦酸锆主体及相应的6种苯胺插层化合物,并进行了元素分析、电感偶合等离子发射光谱(ICP)、X射线粉末衍射(XRD)、红外光谱(FTIR)、激光拉曼光谱(Raman Spectra)、扫描电镜(SEM)、热重分析(TG-DSC)等表征。结果表明6种膦酸锆组成:Zr(O3PCH2)2N(CH2)nCH3·xH2O (n=0,1,2,3,6,9),层间距:1.046～1.962 nm,其结构;带有机侧链的双膦酸连在主体的同一层板上。苯胺插层化合物组成:Zr(O3PCH2)2N(CH2)nCH3·xC6H5NH2·yH2O,层间距:1.097～2.526 nm,苯胺以单分子层排列于主体层间。苯胺聚合反应结果表明聚苯胺并没有包夹在主体层间,而是分散在主体微粒之间。
本文合成了x=1.0的层状晶态和无定形脯氨酸-N-甲基膦(磷)酸锆(分别记为:α-ZLPMPAx=1和ZLPMPAx=1),并进行了相应表征。α-ZLPMPAx=1的组成:Zr(O3PG)(HPO4)·H2O,层间距:1.520 nm,理想结构模型:有机基团与无机基团尽可能均匀地交错排布。通过振荡法、回流法和微波法研究了丁胺(BA)、庚胺(HA)、癸胺(DA)、精氨酸(Arg)、赖氨酸(Lys)、组氨酸(His)等碱性客体分子与α-ZLPMPAx=1主体的插层反应,每个α-ZLPMPAx=1主体分子分别嵌入:0.43 BA、0.34 HA、0.33 DA、0.20 Arg、0.54 Lys和0.39 His。插层化合物α-ZLPMPAx=1-BA、α-ZLPMPAx=1-HA、α-ZLPMPAx=1-DA成功地吸附了酚。
本文合成了4种层状晶态、无定形甘氨酸-N,N-双甲基膦(磷)酸锆(分别记为:α-ZGMDPAx=0.66、α-ZGMDPAx=2、ZGMDPAx=0.66、ZGMDPAx=2),并进行了相应表征。α-ZGMDPAx=0.66、α-ZGMDPAx=2的组成分别为: Zr[(O3PCH2)2NCH2COOH]0.33 (HPO4)1.34·0.70 H2O和Zr[(O3PCH2)2NCH2COOH]·H2O,层间距分别为:1.542和1.271 nm。考察了烷基单胺(甲胺(MA)、乙胺(EA)、丙胺(PA)、BA、HA、DA)、烷基多胺(乙二胺(1E2A)、二乙基三胺(2E3A)、三乙基四胺(3E4A)、四乙基五胺(4E5A)、1,3-丙二胺( PDA))和六氢吡啶(HHP)等客体分子与α-ZGMDPAx=0.66、α-ZGMDPAx=2主体的插层反应。烷基单胺、杂环化合物以双分子层排列于α-ZGMDPAx=0.66主体层间,烷基多胺在α-ZGMDPAx=0.66、α-ZGMDPAx=2主体中产生了多种排列方式。
本文以无定形ZLPMPAx=1、ZGMDPAx=0.66、ZGMDPAx=2为载体制备了固体碱,固体碱强度H-:9.3～15.0,在微波辐射、无溶剂或加热条件下,催化芳香醛与活泼亚甲基化合物的Knoevenagel反应产率:76.4～91.1 %,能重复使用4次以上,是一类环境友好催化剂。ZGMDPAx=0.66固载钯配合物催化Suzuki反应的取代联苯产率:81.4 %。
本文合成了6种不同x值的层状晶态和无定形苄基-N,N-双甲基膦(磷)酸锆(分别记为:α-ZBMDPA、ZBMDPA),并进行了相应表征。α-ZBMDPAx=1.0的组成:Zr[C6H5CH2N(CH2PO3)2]0.5(HPO4)·2.1 H2O,层间距:2.034 nm,其理想结构:层间苯环与苯环相对。详细研究了α-ZBMDPAx=1.0的插层反应性能,成功地将客体分子:烷基单胺(MA、二甲胺(DMA)、三甲胺(TMA)、EA、二乙胺(DEA)、三乙胺(TEA)、PA、BA、二丁胺(DBA)、三丁胺(TBA)、HA、DA)、烷基多胺(1E2A、2E3A、3E4A、4E5A、PDA)、杂环化合物(四氢吡咯(TPR)、HHP、吗啉(ML)、哌嗪(PH))嵌入层状化合物α-ZBMDPAx=1.0层间,烷基单胺、杂环化合物在α-ZBMDPAx=1.0主体层间单分子层排列并与主体层板倾斜成一定角度,烷基多胺也有多种排列方式。插层化合物α-ZBMDPAx=1.0-BA\α-ZBMDPAx=1.0HA、α-ZBMDPAx=1.0-DA成功地吸附了酚,α-ZBMDPAx=1.0-3E4A、α-ZBMDPAx=1.04E5A吸附了甲醛。
本文合成了无定形ZBMDPA载体固载多胺(1E2A、2E3A、3E4A、4E5A)配体及4种钯配合物,进行了FTIR、原子吸收光谱(AAS)、X射线光电子能谱(XPS)、XRD等表征,苄基-N,N-双甲基膦(磷)酸锆多胺配体固载钯配合物催化卤代芳烃与芳基硼酸的Suzuki反应,结果表明碘代芳烃偶联反应产率:92.1 %,催化剂与产物分离容易,催化剂能重复使用5次以上,而对溴代芳烃和氯代芳烃催化活性较低。本文通过微波辐射、超声波震荡、回流法等研究了His、Arg、Lys与α-Zr(HPO4)2·H2O(α-ZrP)的超分子插层组装,这些客体以单分子层排列在α-ZrP主体层间,每个α-ZrP分子分别嵌入:0.50 His、0.13 Arg和0.84 Lys。插层化合物α-ZrP-His对水相中丙酮与4-硝基苯甲醛Aldol反应具有一定的催化活性和一定的重复使用性,是一类值得进一步研究的多相催化材料。
It is very important to study synthesis, characterization, intercalation and catalysis of zirconium phosphonates and hybrid zirconium phosphates for host-guest supermolecule chemistry, property, preparation, application and development of multifunctional materials.
In this paper, 10 kinds ofα-aminomethylphosphonic acid derivitives were synthesized by the Mannich-type reaction. The property and structure ofα-aminomethylphosphonic acid derivitives were characterized and discussed by elemental analysis, Fourier Transform Infrared Transmission-absorption Spectra (FTIR), Nuclear Magnetic Resonance (1H NMR and 31P NMR) in detail.
12 kinds of layered zirconium dimethylphosphonates and aniline intercalation compounds were synthesized and characterized by elemental analysis, Inductive Coupled Plasma Emission Spectrum (ICP), X-ray Powder Diffraction (XRD), FTIR, Laser Raman Spectra (Raman Spectra), Scanning Electron Microscope (SEM), Thermogravimetry and Differential Scanning Calorimetry (TG-DSC). The results demonstrated that the compositions of zirconium phosphonates were Zr(O3PCH2)2N(CH2)nCH3·xH2O (n=0, 1, 2, 3, 6, 9) with the interlayer distances of 1.046 nm to 1.962 nm, two dimethylphosphonates might bind to the same layer. The compositions of aniline intercalation compounds were Zr(O3PCH2)2N(CH2)nCH3·xC6H5NH2·yH2O with the interlayer distances of 1.097 nm to 2.526 nm, and anilines arranged as monomolecular layers in the gallery of these hosts. The polymerization of aniline showed that polyaniline was not inserted between the layers of host, but diffused in the particles of host.
2 kinds of layered crystalline and amorphous zirconium proline-N-methylphosphonate-phosphates (α-ZLPMPAx=1 and ZLPMPAx=1) were synthesized and characterized by the above methods, the results indicated that the composition ofα-ZLPMPAx=1 was Zr(O3PG)(HPO4)·H2O with the interlayer distance of 1.520 nm, the N-methylproline groups and P-OH arranged alternatively. The intercalations of butylamine (BA), heptylamine (HA), decylamine (DA), arginine (Arg), lysine (Lys) and histidine (His) withα-ZLPMPAx=1 host had been studied by shaking, refluencing and microwave irradiation, 0.43 BA, 0.34 HA, 0.33 DA, 0.20 Arg, 0.54 Lys and 0.39 His inserted into in the gallery of one moleculeα-ZLPMPAx=1 host, respectively. The intercalation compoundsα-ZLPMPAx=1-BA,α-ZLPMPAx=1-HA andα-ZLPMPAx=1-DA had successfully adsorbed phenol, 4-chlorophenol and 2,4-dichlorophenol.
4 kinds of layered crystalline and amorphous zirconium glycine-N,N-dimethylphosphonate-phosphate (α-ZGMDPAx=0.66,α-ZGMDPAx=2, ZGMDPAx=0.66 and ZGMDPAx=2) had been prepared and characterized by the above methods. The compositions ofα-ZGMDPAx=0.66 andα-ZGMDPAx=2 were Zr[(O3PCH2)2NCH2COOH]0.33 (HPO4)1.34·0.70 H2O and Zr[(O3PCH2)2NCH2COOH]·H2O, the interlayer distances of them were 1.542 nm and 1.271 nm, respectively. It was found that the intercalations of alkylmonoamines (methylamine (MA), ethylamine (EA), propylamine (PA), BA, HA, DA), polyamines (ethylenediamine (1E2A), diethylenetriamine (2E3A), triethylenetetramine (3E4A), tetrathylenepentamine (4E5A), 1,3-propyldiamine (PDA)), hexahydropyridine (HHP) withα-ZGMDPAx=0.66 andα-ZGMDPAx=2 hosts, alkylmonoamines and heterocyclic compounds arranged as bimolecular layers in the gallery ofα-ZGMDPAx=0.66, polyamines formed multi-array in the gallery ofα-ZGMDPAx=0.66 andα-ZGMDPAx=2.
The solid bases with H-=9.3 to 15.0 were prepared by the amorphous supports ZLPMPAx=1, ZGMDPAx=0.66 and ZGMDPAx=2. The Knoevenagel condensations of aromatic aldehydes with active methylene compounds were catalyzed by the solid base in yield of 76.4 % to 91.1 % under microwave irradiation and solvent-free, or heating, the solid base could be reused four times. The solid base is a new type of environmentally benign catalyst. On the meanwhile the palldium complex supported on ZGMDPAx=0.66 exhibited a yield of 81.4 % for Suzuki cross-coupling reaction.
6 kinds of layered crystalline and amorphous zirconium benzyl-N,N-dimethylphosphonate-phosphates (α-ZBMDPA, ZBMDPA) were also prepared and characterized by the above methods. The composition ofα-ZBMDPAx=1.0 with the interlayer distance of 2.034 nm was Zr(HPO4)(C6H5CH2N(CH2PO3)2)0.5?2.1 H2O, and two phenyl ofα-ZBMDPAx=1.0 double layers faced to face each other. Alkylmonoamines (MA, dimethylamine (DMA), trimethylamine (TMA), EA, diethylamine (DEA), triethylamine (TEA), PA, BA, dibutylamine (DBA), tributylamine (TBA), HA, DA), polyamines (1E2A, 2E3A, 3E4A, 4E5A, PDA), heterocyclic compounds (pyrrolidine (TPR), HHP, morpholine (ML), piperazine(PH)) had successfully inserted into the gallery ofα-ZBMDPAx=1 host, alkylmonoamines and heterocyclic compounds arranged as monomolecular layers in the gallery ofα-ZBMDPAx=1, polyamines also formed multi-array in the gallery of.α-ZBMDPAx=1. The intercalation compoundsα-ZBMDPAx=1-BA,α-ZBMDPAx=1-HA andα-ZBMDPAx=1-DA adsorbed phenol, 4-chlorophenol and 2,4-dichlorophenol,α-ZBMDPAx=1-3E4A andα-ZBMDPAx=1-4E5A adsorbed formaldehyde.
Series of pallidum complexes were prepared by introducing the ligand polyamines (1E2A, 2E3A, 3E4A and 4E5A) into the support ZBMDPA. These pallidum complexes supported on ZBMDPA polyamines were characterized by FTIR, Atomic Absorption Spectra (AAS), X-ray Photoelectron Spectra (XPS) and XRD. The pallidum complexes catalyzed Suzuki cross-coupling reaction of aryl halides with aryl boronic acids, compared with aryl bromides and aryl chloride, aryl iodide obtained better yield (92.1%), the catalyst could be easily recovered and reused more than five times.
In addition, the intercalations of His, Arg, Lys withα-Zr(HPO4)2·H2O (α-ZrP) had been studied under microwave irradiation, ultrasound and refluencing, these amino acids arranged as monomolecular layers, 0.50 His, 0.13 Arg and 0.84 Lys inserted into the gallery of one moleculeα-ZrP, respectively. The intercalation compoundα-ZrP-His catalyzed Aldol reaction of acetone with 4-nitrobenzaldehyde in proper yield and could be reused. It is necessary to researchα-ZrP-His as multiphase catalysis materials.
引文
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