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Table of Content
24 December 1992, Volume 8 Issue 4
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Articles
A Study of Acidic Sites in H[M]-ZSM-5 Zeolites by XPS, IR and TPD
XTAO Feng-shou, XU Ru-ren, XU Yi-hua, WEI Quan
1992, 8(4): 337-342.
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The present paper covers an X-ray photoelectron spectroscopic (XPS) method proposed for identifying Bronsted and Lewis acidic sites in zeolites and estimating acidic strength of these sites. It was found that the adsorption of pyridine on different acidic sites of H[M]-ZSM-5 zeolites exhibited three peaks: A(402.20-401.30 eV), B(400.95-400.40 eV) and C(399. 40-399. 10 eV). The peaks Aand Bare assigned to the N
1x
level of pyridine adsorbed on Bronsted and Lewis acidic sites, and peak Cis assigned to the N
1x
level of pyridine adsorbed on a weak Lewis site and/or strongly physisorbed pyridine, respectively. The comparison of the ratio of the Bronsted and Lewis acidic sites determined from the relative intensities of the N
1x
, peaks with IRspectroscopic data shows that there is an inhomoge-neous distribution of Bronsted and Lewis acidic sites in H[M]-ZSM-5 zeolites.
Synthesis and Characterization of Heteropolytungstosilicate Complexes with the Lanthanide Elements
WANG Zhan-wen, WU Nai-jun, WANG Shu-fang
1992, 8(4): 343-347.
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Lanthanide heteropoly compounds K
15
[Ln(HSiW
9
O
34
)
2
]·28H
2
O(Ln=La, Ce, Nd), denoted as Ln(SiW
9
)
2
, were synthesized and characterized by element analysis, TG-DTA, IR, UV, XPS and XRD. The results show that partial oxygen in Ln(SiW
9
)
2
was coordinated with Ln
3-
, where Ln
-3
was in the inner side of the heteropoly anions, while the fundamental structure of SiW
9
had little change. The result was supported by ion exchange experiment.
Activity and Selectivity in CO Hydrogenation with Silica-supported Ru-Co Bimetallic Cluster-derived Catalysts
XIAO Feng-shou, XU Ru-ren, Fukuoka A., Ichikawa M.
1992, 8(4): 348-354.
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The catalytic performance of bimetallic Ru-Co catalysts prepared from a series of H
3
Ru
3
Co(CO)
12
. RuCo
2
(CO)
11
and HRuCo
3
(CO)
12
in CO hydrogenation was investigated, and it was found that the Ru-Co bimetallic carbonyl cluster-derived catalysts showed a high activity for products, particularly higher oxygenates, compared with the catalysts prepared from impregnation or co-impregnation of monometallic clusters such as [HRu
3
(CO)
11
] and Co
4
(CO)
12
The selectivity for oxygenates in CO hydrogenation highly increased with the molar ratio of Co/Ru in the Ru-Co bimetallic cluster to CO/H
2
in feed gas. Raising reaction temperature led to an intensive increase of CO conversion and a considerable decrease of selectivity for oxygenates. In situ FT-IRstudies revealed that the band at 1584 cm
-1
on Ru-Co bimetallic cluster-derived catalysts at 453 Kunder syngas (CO/H
2
=0. 5) has a good linear relationship to rates of oxygenate formation.
Studies on the Synthesis and Properties of K
8
[TiP
2
W
17
O
62
]·12H
2
O
LIU Shi-zhong, CHENG Yi, FANG Guang-rong, ZHOU Jian-gang
1992, 8(4): 355-359.
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The present paper covers a salt of 2:18 heteropoly complex of tungstotitanophosphate prepared with the method of improved sequence preparation. The title compound was characterized by elemental analysis,
31
PNMR spectra, polarography, cyclic voltammetry, IR, UV, X-ray powder diffraction, X-ray photoelectron spectra and TG-DTAanalysis. The results show that the complex with the formula K
8
[TiP
2
W
17
O
62
]·12H
2
O has Dawson structure. Its properties such as spectra, redox behavior and thermal stability are discussed.
Investigations on the Chemiluminescence Reaction Between Luminol and Reductant
LU Jiu-ru, ZHANG Xin-rong, FENG Man-lian, ZHANG Jian-qiang, ZHANG Zhu-jun
1992, 8(4): 360-364.
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The chemiluminescence reaction between luminol and reductant was investigated by a flow-injection system. The results show that this reaction can be used for the determination of the reductant which is active to chemiluminescence in alkaline lumminol, and of the substance which can, in appropriate manner, be converted into the active reductant. The mechanism of the chemiluminescence reaction may be that the reductant reduces dissolved oxygen to O
2
, then O
2
reacts with alkaline luminol to generate chemiluminescence.
Studies on Tricyclohexyltin (Ⅳ) Diaryldithiophosphates
XIE Qing-lan, LUO Ning, LI Jing, JING Xu-ying
1992, 8(4): 365-369.
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Fourteen new tricyclohexyltin (Ⅳ)-O,O-diaryldithiophosphates were synthesized and determined by IR,
1
HNMR,
13
CNMR,
119
Sn NMR MS, and elemental analysis. The structures of all the compounds consist of discrete molecule containing a four-coordinated tin atom. Results from the preliminary biological test show that these compounds have a high miticidal activity.
Reaction of Substituted Cyclopentadienyl-magnesium-Chloride with Carbonyl Compound (Ⅰ)--Reaction of (1, 1-Dialkyl-3-Butenyl) Cyclopentadienyl-magnesium-chloride with Ketones
LI Ji-hai, LIU Jin-ting, JIAO Lun-ji, ZHANG Xiao-qing, MA Yu-dao, ZHANG Nan
1992, 8(4): 370-376.
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The substituted cyclopentadienyl-magnesium-chloride, obtained by exocyclic addition of 6,6-dialkylfulvene and allyl-magnesium-chloride, reacted with the ketone 3, the product was hydrolyzed and dehydrated to give the 2-(1,1-dialkyl-3-butenyl)-6,6-dialkyl-fulvene 5. The structure of 5 was determined by using the
1
HNMR spectra of 5 and the adducts of 5 with tetracyanoethylene.
Synthetic Studies on 1-Amino-1-Cyclopropane-Carboxylic Acid(Ⅰ)--The Cyclopropanation via Addition-Elimination Reactions
ZHANG X. A., Campbell M. M., Brown, D. W.
1992, 8(4): 377-381.
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Various addition-elimination approaches have been explored for diastereoselective construction of 1-amino- 1-cyclopropane-carboxylic acid (ACPC) derivatives, and the desired product was obtained from a reaction of cyclo(NAc-L-Val-NAc-Gly) and methyl α-bro-moacrylate under protonic solvent.
Synthesis, Structure and Properties of (n-Bu
4
N
3
[Mo
6
O
18
NNAr(NO
2
)
2
]
WANG Shuang-xi, WANG Xin, ZHAI Ying-li
1992, 8(4): 382-387.
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The title compound was synthesized and characterized by means of elemental analysis, IR, DTA-TG and UV. Its single crystal structure was solved by using direct methods. The compound crystallizes in the orthorhombic space group P
mcR
with lattice parameters: a=1. 7261(2), b=l. 7537(3), c=2. 4258(3) nm. V=7. 34220 nm
3
, F(000)=3648, Z=4. The structure was refined to conventional discrepancy factors of R=0. 060 for 3176 observed reflections [Ⅰ>3σ/(Ⅰ)]. The anion represents a modification of the well-known [Mo
6
O
19
]
2-
anion, in which a single terminal oxo group is replaced by a 2,4-dinitrophenyl hydrazine ligand while the structure integrity of the hexanuclear framework is maintained.
Studies on the Response Dynamics of a Gas-Sensing Membrane Probe
LI Fan-chao
1992, 8(4): 388-394.
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The present paper covers the response dynamics of a gas-sensing membrane probe, which is described by the dynamic differential equation based upon a steady-state diffusion process. The theoretical results indicate that the response time is dependent upon membrane properties, membrane geometry, internal electrolyte composition, the dissociation constant of the conjugate reaction, the initial gas concentration in the internal electrolyte, and the gas concentration in the evaluation sample. The theoretical prediction is in good agreement with the experimental result. Amethod for determining a gas-sensing probe' s dynamic parameter is proposed in this paper also.
X-Ray Photoelectron Spectroscopic Study on the Synthesis of Copper Sulphide in LB Films(Ⅱ)
CHEN Hui-juan, CHAI Xiang-dong, WEI Quan, JIANG Yue-shun, LI Tie-jin
1992, 8(4): 395-398.
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The present paper covers the formation process of copper sulphide in copper stearate Langmuir-Blodgett films studied carefully by XPS. The further identification of sulfur species and the examination of its change in the reaction have been made. Also the formation mechanism of sulfur species in the special microenvironment-LB films is discussed.
Structure of Palladium(Ⅱ) Complex with 2-Hydroxy-propane 1, 3-diamine-N,N,N',N'-tetraacetic Acid
SONG Rui-fang, ZHANG Cun-zhi, LI Fei, JIN Song-chun, JTN Zhong-sheng
1992, 8(4): 399-404.
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The reaction of PdCl
2
in water with 2-hydroxypropane-1, 3-diaminetetraacetic acid (HPDTA) gave the complex Pd (C
11
H
16
N
2
O
9
)·1. 5H
2
O, which was characterized by elemental analysis, IR, NMR and single-crystal X-ray diffraction. The spectroscopic and X-ray diffraction data show that Pd (Ⅱ) is coordinated by two nitrogen atoms and two car-boxylic oxygen atoms. The complex crystallizes in monoclinic space group P
c
with a=1. 1240(2), b=1. 1183(2), c=1. 2597(3) nm, β=96. 33(2)°V=1. 5737(6) nm
3
, Z=4, R=0.038. The structure contains two crystallographically independent molecules which have slightly different orientations and are connected by hydrogen bonds.
The Numbers of Configurations, Chiral and Achiral Configurations of Saturated Polybasic Alcohols Containing an Adamantane Skeleton
WANG Jian-ji, LIU Xin-hua, WANG Xi-gui
1992, 8(4): 405-409.
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By using Polya' s theorem, the generating functions of configurations, chiral and achi-ral configurations of saturated polybasic alcohols containing an adamantane skeleton were obtained. Tn order to calculate the generating functions of compounds which are substituted with a limited condition, an exclusive method is used and cycle index is modified.
Quantum Chemical Studies on Polydecker Sandwich Compounds with C
3
B
2
H
5
Ligand
HUANG Yuan-he, XIE Qian, LIU Ruo-zhuang
1992, 8(4): 410-414.
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The results of SCF CNDO-CO calculation on polymeric [(η
5
,μ-2,3-dihydro-1, 3-di-borolyl)M](M=Cr, Mn, Fe, Co, Ni) indicate that polydecker sandwich compounds with odd valence electrons in each stacking unit (C
3
B
2
H
5
)M have Peierls distorted structures, while those with even valence electrons are favorable to the formation of regular structures. The Band structures show that both LUand HObands are d-bands for all of the polydecker sandwich compounds studied.
Ab Initio
Calculations on Nitramide and Its Methyl Derivatives(Ⅱ)--The Harmonic Force Fields and Vibrational Spectra of Nitramide and Its Isotopic Derivatives
FAN Kang-nian, WANG Wen-ning, XTAO He-ming, LI Yong-fu
1992, 8(4): 415-421.
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The harmonic force field and the vibrational spectrum of nitramide were calculated by using the ab initio gradient program TEXA Sat the Hartree-Fock level with a 4-21G basis set. The directly computed theoretical harmonic force field was scaled by using empirical scale factors which are transferred from other molecules and provided an a priori prediction of fundamental frequencies and intensities. The average deviations between predicted vibrational frequencies of nitramide and experimental IRspectrum in an argon matrix are 63 cm
-1
for symmetric vibrations and 41 cm
-1
for antisymmetric modes. Anew set of scale factors was optimized in this paper. These scale factors reduced the average deviations to 2. 3 cm
-1
for symmetric modes and 0. 8 cm
-1
for antisymmetric ones. The vibrational spectra of three isotopic derivatives of nitramide were predicted by using the force field resulted from the optimized set of scale factors, which are in good agreement with their experimental data in an argon matrix.
Reaction Ergodography and Transition State Analyses of the Addition of AIH
3
to Acetylene
SU Zhong-min, HUANG Jing-an, ZHAO Cheng-da
1992, 8(4): 422-427.
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The present paper covers the reaction ergodography for the addition of AlH
3
to acetylene investigated by ab initio calculation with RHF/3-21G basis set. The changes in some physical properties along the reaction path (IRC) are presented. The formations of FMOs of the transition state have been analyzed according to the Fukui' s method. On the basis of the perturbation theory and Wolfsborg Helmholtz formula, we calculated the FMO' s energy orders of TSand its formation that shows the HOMO of TSconsists of LUMO, HOMO of AlH
3
and HOMO of HCCH.
Synthesis and Self-Assembly Properties of Single-Chain Amphiphiles Containing Schiff Base Chromophore
WU Li-xin, LI Guo-wen, LIANG Ying-qiu
1992, 8(4): 428-431.
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A series of single-chain amphiphiles containing Schiff base moiety(CnSchC
4
N
+
, n=4, 7, 10, 12, 16) were synthesized. The self-assembly properties were investigated by
1
HNMR spectra, DSC and EM for aqueous solutions of these samples. The aggregates, vesi-cles, were formed when n=7. The influence of additional group-O-is discussed.
Kinetics and Mechanism of Oxidation of Glycol by Dihydroxydiperiodatonickelate (Ⅳ)Complex in Aqueous Alkaline Medium
WANG An-zhou, LI Feng-mai, LI Zhi-ting, DING Tian-hui, SHAN Jin-huan
1992, 8(4): 432-438.
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The kinetics of oxidation of glycol by dihydroxydiperiodato nickelate (Ⅳ) complex (DDN) was studied by spectrophotometry in aqueous alkaline medium in a temperature range of 25-40℃. The reaction was found to be first order with respect to Ni(Ⅳ) and also to be first order with respect to glycol. The rate increases with the increase in [OH ] and decreases with the increase in [IO
4
-
], showing that dihydroxymonoperiodatonickelate (Ⅳ)(DMN) is the reactive species of oxidant. Salt effect indicated that the reaction is of ion-dipole type. No free radical was detected. Amechanism of an inner-sphere two-electron transfer reaction involving a preequilibrium between DDN and DMN is proposed, and the rate equation derived from the mechanism can explain all experimental observations. Activation parameters of the rate-determing step and the equilibrium constants were calculated.
Silica-supported Polysiloxanes with Dithiacrown Ether Groups and Their Platinum Complexes
CHEN Yuan-yin, LU Xue-ran, SONG Xiao-ping
1992, 8(4): 439-444.
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The present paper represents the syntheses of polypropyloxymethyldithia 15-crown-5 and 18-crown-6 supported on silica and their platinum complexes. The platinum complexes are effective catalysts for the hydrosilylation of olefins with triethoxysilane. The influences of temperature, amount of platinum complexes used and the nature of olefins used on the catalytic activity of the complexes are also investigated in this paper.
Diffusion Studies on Polystyrene in 1,4-Dioxane
LT Jun-bai, MA Rong-jiu, WANG Jing-jiang, SHEN Jia-cong
1992, 8(4): 445-449.
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The diffusion behavior of polystyrene with narrow molecular weight distribution at 20℃ in 1, 4-dioxane was investigated by the photon correlation spectroscopy. The cumulant method was employed for the analysis of the intensity-intensity autocorrelation function measured over a wide range of the scattering vector. The diffusion coefficient D was determined as the function of concentration Cin the molecular weight range of 3. 0×10
4
-1. 20×10
6
. In a low concentration range, D was found to be linearly dependent on C, which has been found for some other systems. The dependence of Don molecular weight at infinite dilution can be written as an empirical formula D
0
=k
D
M
M
-γ
, the exponent γ(0. 576 ±0. 01) is in good agreement with the result of the scaling theory.
Photopolymerization of Cyclohexene Oxide Initiated with Iron-arene Complex
CHEN Yong-lie, CHEN Xu-dong, LIANG Zhao-xi
1992, 8(4): 450-453.
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)
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Two iron-arene complex photoinitiators with different substituents in arene ligands were synthesized, their activities in initiating photopolymerization of cyclohexene oxide (CHO) were compared with that of IRGACURE 261, a commercialized photoinitiator from Ciba-Geigy. Ahigher activity was found when the arene ligand was substituted with a stronger electron donating group. For the system initiated by IRGACURE 261 the concentration of active centers in CHOpolymerization was determined and it was found that the concentration is maximum at around 35℃. The post (dark) polymerization was significant, the polymerization yield decreased with the increase of irradiation temperature and increased with the increase of post polymerization temperature. The results are interpreted based on the mechanism proposed by Lohse, et al..
The Effect of Synthesis Method on Three-component IPNs Morphology and Property
WANG Jing-yuan, LI Yu-wei, TANG Xin-yi, JING Gui-pinfe, SHUN Gui-fen, YANG Yu-hua
1992, 8(4): 454-460.
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Three-component IPNs were synthesized from polyurethane/poly (methyl acrylate aminoethyl methacrylate)/epoxy resin [PU/P(MADMA)/EP] by simultaneous synthesis interpenetrating polymer networks method(SINs) and sequential synthesis interpenetrating polymer networks method (STPNs). Comparing the effect of the two synthesis methods on the morphology and mechanical properties of three-component IPNs, it was found that the compatibility of three-component IPNs depends on the component ratios and interpenetrating formation, the different synthesis methods make the entanglement and interpenetrating between networks changed. The tensile strength of SIPNs is bigger than that of SINs, while the elongation at break of SINs is bigger than that of SIPNs. It is feasible to use stepwise staining method to observe the morphology change.
Studies on the Gold-Coated Electrode with Grid
ZOU Ming-zhu, SHENG Gui-hua, ZHENG Guo-dong, ZHFNG Yan-sheng
1992, 8(4): 461-464.
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Introduction Thin-layer spectroelectrochemical method has many unique advantages, therefore this method has been widely applied and developed. Recently light transparent thinlayer spectroelectrochemical cells with various types of structures have been reported at home.
Application of Microwave Heating Technique to Esterification
LIU Fu-an, XU Wen-guo, LI Yao-xian
1992, 8(4): 465-467.
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)
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Introduction Although the application of microwave technique has been reported as a new type of energy source chemically, it is only in recent years that this technique has been used as the energy source for organic synthesis. In 1986, R. Gedye, et al., published the report of the benzoate synthesis from the respective reactions between benzene carboxylic acid and methanol, propanol or butanol under microwave heating and the catalysis of H
2
SO
4
.
Reductive Desulfurization of Thioamides to Amines by Catalytic Hydrogen Transfer Reaction
YOU Qi-dong, ZHOU Hou-yuan, WANG Qi-zhuo, LEI Xing-han
1992, 8(4): 468-472.
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Introduction Reductive desulfurization of thioamides to amines is one of the methods to prepare amines and is generally achieved by a) Zn in acid, b) sodium or aluminum amal- gams, c) lithium alumminium hydride, d) Raney Ni and e) electrolytic reduction. These methods are not very convenient to be operated and some need more complex instrument. Here is reported the reductive desulfurization of thioamides to amines by catalytic hydrogen transfer reaction(CHT).
Nucleophilic Substitution of Halogenonitrobenzenes by Electrogenerated O
2
-
on Carbon Gas-diffusion-electrode
WANG Shu-fang, HUANG Chu-bao, ZHANG Dong
1992, 8(4): 473-476.
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)
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Introduction The electrochemical reduction of O
2
was investigated widely during the past two decades. O
2
-
can react with various organic compounds. O
2
-
as a new synthesis reagent has been being explored.
Preparation of the In
2
O
3
·Sn Films by MO-CVD Technique
LUO Wen-xiu, REN Peng-cheng, TAN Zhong-ke, LI Zhi-ping
1992, 8(4): 477-479.
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Introduction In
2
O
3
·Sn films have high transparency(>95％) within the visible spectral region, low resistivity(10
-2
-10
-4
ohm·cm) at room temperature and superior thermal stability. These films have been applied to solar cells, electronics and photoelectronics fields. In recent years, organometallic-CVD method has emerged as a successful alternate to the physical methods and general CVDfor the growth of these films.
A Theoretical Studies on the Thermolysis Mechanism of α-Aminonitrile
HONG San-guo, LI Fu-quan, FU Xiao-yuan
1992, 8(4): 480-482.
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Introduction α-Aminonitrile(or aminoacetonitrile) is a kind of reactive bioorganic molecules, and it may exist in insterstellar clouds. its importance lies in that a-aminonitrile may play a role in the generation of large carbon-nitrogen chain molecules. By means of flash vacuum thermolysis and gas-solid reaction (FVT-GSR) tech-nique, Guillemin, et al., studied the thermolysis of a-aminonitrile.
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