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中文
Table of Content
24 June 1990, Volume 11 Issue 6
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Articles
A Study on Ternary System of LaCl
3
-Am(Am=Gly, Glu, Ser)-H
2
O(25℃)
Chen Juxiang, Ran Xinquan, Guo Zhizhen, Chen Yunsheng
1990, 11(6): 555-560.
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Three systems of LaCl
3
-Am-H
2
O(Am=Gly, Glu, Ser) were strudied. Solubilities and refraction indices of saturated solutions of these systems were measured at 25±0. 05℃ and corresponding equilibrium diagrams were constructed. In these systems there are 4 ternary complexes-La(Gly)Cl
3
·2H
2
O(A
1
), La(Gly)
3
Cl
3
· 3H
2
O(A
2
), La
2
(Glu)
3
Cl
6
· 8H
2
O(C), La(Ser)Cl
3
· 3H
2
O (E). The complexes are not yet found in literatures except(A
2
), and they were characterized by molar conductivity, IR spectra, X-ray diffraction, Thermogravimetric and differential analysis.
Synthesis of Poly-4-oxa-6,7-bis(diphenylphosphino) heptyl Siloxanc Rhodium Complex and Its Catalytic Hydrosilylation Behavior
Lu Xueran, Zhong Zhenlin, Chen Yuanyin
1990, 11(6): 561-564.
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Poly-4-oxa-6,7-bis(diphenylphosphino)heptyl siloxane rhodium complex was synthesized from 4-oxa-6,7-dichloroheptene-1 via hydrosilylation with trimethoxysilane in the presence of tetrakis (triphenylphosphine)platinum complex as the catalyst, phosphatization with potassium diphenylphos-phide, sequentially, followed by immobilization on fumed silica and then the reaction with rhodium chloride. It exhibited good catalytic activity for the hydrosilylation of olefins, such as decene, do-decene, w-chloroundecene, phenyl allyl ether, allyl benzene, allyl glycidyl ether, styrene, and methyl methacrylate, etc., with triethoxysilane at 90℃. Apossible structure pattern of this silicone-supported bidentate phosphine rhodium complex has been suggested.
Studies on Rare Earth Coordination Compounds with Crown Ether (ⅩⅦ) )——Syntheses and Properties of Rare Earth Coordination Compounds of Schiff Base Macrocyclic Ligand
Lei Xiubin, Ji Zhenping, Xiao Wenjin
1990, 11(6): 565-568.
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Fifteen lanthanoid complexes of Schiff base Lmacrocyclic ligand were prepared by template reactions. Their compositions and structures were characterized by elemental analysis, IR, UV spectra and electrical conductance measurement. The stability of complexes was studied by DTA-TG analyses, and L macrocyclic ligand was synthesized in order to compare it with the complexes.
Studies on the Mechanism of the Catalytic Prewave of Eu( Ⅲ )-o-Phcnanthroline
Gao Xiaoxia, Hu Tao
1990, 11(6): 569-573.
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The polarographic catalytic prewaves of metal complexes have been used successfully for determining small quantities of non-electroactive species, an outstanding example for the determination of metals is the AC polarography of Eu-v-phenanthroline. The reaction mechanism of this prewave are examined by many electrochemical experiments such as AC polarography, differential pulse polarography, electrocapillary curves, cyclic voltammetry, etc. A ligand-bridge mechanism is then suggested in comparison with the formation of electroactive complexes in the case of Co ( Ⅱ ) or Ni ( Ⅱ ) with o-phenanthroline.
Studies on the Mechanism of Polarographic Catalytic Prewaves of Co( Ⅱ ) and Ni( Ⅱ ) with o-Phenanthroline
Hu Tao, Gao Xiaoxia
1990, 11(6): 574-578.
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In comparison with the ligand-bridge-mechanism of Eu( Ⅲ )-o-phenanthroline prewave suggested in our previous paper(4), the mechanism of prewaves of Co( Ⅱ ) and Ni( Ⅱ ) with o-phcnan-throline is further investigated by several electrochemical techniques such as ACpolarography, differential pulse polarography, cyclic voltammetry and ultraviolet spectrophotometry, etc. It has been shown that Co( Ⅱ ) and Ni(Ⅱ) form complexes with o-phenanthroline in NH
4
Ac solution at pH 7 and 4, respectively. The complexes are adsorbed on the surface of mercury electrode, on which o-pncnan-throline is also adsorbed. The prewaves in the form of sharp, reversible AC polarograms and cyclic voltammograms can be used to determine micro amounts of Co and Ni and also o-phenanthroline. From the results of the experiments it may be concluded that the mechanism of both the Co( Ⅱ ) and Ni( Ⅱ ) prewaves is an electroactive complex mechanism with some differences between them.
Studies on A. C. Oscillopolarogram (Ⅳ ) ——The Incision
Bi Shuping, Gao Hong(H. Kao)
1990, 11(6): 579-582.
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The properties of oscillopolarographic incision was studied and theoretical conclusions were confirmed by experimental results.
Studies on Oscillopolarographic Titration Involving Cupferron
Xu Hongding, Liu Zaixin, Wang Minghui
1990, 11(6): 583-585.
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In this paper, the analytical methods for determining cupferron with a standard copper solution or copper in alloy with standard cupferron by oscillopolarographic titration have been presented. The methods are rapid and accurate, and the end point is sharp. Satisfactory results can be obtained for determination of copper in copper alloy. The variation coefficients are 0. 07%～0. 17%. The kinetic behaviour of the cupferron in the instance of ultraviolet irradiation has also been studied.
Studies on 1,4-Bis(Phenyl Ethynyl)Benzene and Its Bis Substituted Phenyl Derivatives
Huan Zhenwei, Tang Jiansheng, Kao Zhenheng
1990, 11(6): 586-590.
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1, 4-Bis(phenyl ethynyl) benzene and its bis substituted phenyl derivatives were synthesized. Their fluorescence quantum yields, laser energy transfer efficiencies, Infrared spectra, and Raman spectra have been measured. The majority of the Infrared bands and Raman bands of the title compounds have been assigned. Their structures and the effect of substituents on the both spectra have been discussed.
ESR Study of Free Radical Intermediates Formed During the Electrode Process (Ⅳ)——Electrolysis-oxidation of Some Alkylamine
Liu Yang, Xu Guangzhi, Sha Jinggui
1990, 11(6): 591-594.
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Active free radicals formed in the process of electrolysis-oxidation of some alkylamine (trimethylamine, triethylamine, tri-n-propylamine, tri-i-octylamine, diethylamine and hexahydropy-ridine) were studied by the combination of ESRspectrometry and spin trapping technique. The results show that not only the secondary a-Ccenter radical formed in the anode chamber but also cathodic H atom can be trapped by spin trapping reagent phenyl-t-butyl nitrone.
Syntheses and Properties of Schiff Base Type and Secondary Amine Type Bis-Crown Ethers
Zhang Zheng, Zhu Chunsheng, Cao Jianguo, Wang Zhilin
1990, 11(6): 595-599.
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Reaction of 2-HOC
6
H
4
CHO with X-R-X [R=- CH
2
CH
2
-, - (CH
2
)
3
-, - (CH
2
)
4
-, -(CH
2
)
6
-, -CH
2
CH
2
(OCH
2
CH
2
)
2
-, X=Br, p-CH
3
C
6
H
4
SO
3
-] in the presence of K
2
CO
3
in DMF gave 2-OHC-C
6
H
4
-OROC
6
H
4
CHO-2, which were condensed with 4'-aminobenzo-15-crown-5 to give five new schiff base type bis-crown ethers. Reduction of these schiff bases with LiAlH
4
gave secondary amine type bis-crown ethers. Results of conductivity measurement showed that these bis-crown ethers formed 2 : 1 (crown ether : metal ion) sandwich type complexes with potassium, rubidium chlorides or formed 1 : 1 complexes with sodium ion. In addition, the bis-crown ethers were used as an active substance in PVC membrane potassium ion selective electrodes, and the liner range, selective coefficient were also measured.
The stereoselective Synthesis of Insect Sex Pheromone of Z- and E-Alken-1-yl Acetates via Organoboranes
Zhao Dejie, Lu Kui, Xu Yuexing, Zhang Guomjn
1990, 11(6): 600-604.
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The hydroborating agnet, monobromoborane-dimethyl sulfide(H
2
BBr · SMe
2
) 2b, was prepared from the reaction of borane-dimethyl sulfide(H
3
B · SMe
2
) with carbon tetrabromide in the molar ratio 1 : 1 at 60℃ for 20 h. Some insect sex pheromones with Z- and E-7-alken-l-yl acetate have been prepared by Zweifel's cis- and trans-olefine synthesis. Monohaloborane-dimethyl sulfide(H
2
BX · SMe
2
,X = Cl,Br) 2 hydroborates terminal alkenes rapidly and quantitatively to give dialkylhalobo-ranes 3 at room temperature. Dialkylboranes 4, prepared in situ via reduction of 3 with LiAlH
4
, hy-droborate 2-(7-octyn-l-yloxy-)tetrahydropryan 5 and 2-(8-bromo-7-octyl-1-yloxy-)tetrahydropy-ran 6 to provide B-(trans-1-alkenyl)dialkylboranes 7 and B-(cis-1-bromo-1-alkenyl)dialkylboranes 10 respectively. Treatment of 7 with iodine in the sodium methoxide at -78℃ forms the corresponding cis-disubstituted alkenes 8, followed by the acetylation to give Z-7-alken-1-yl acetates 9. Treatment of 10 with sodium methoxide at 0℃ provides B- (trans-1-alkyl-1-alkenyDalkylborinate esters 11, which on protonalysis produce the E-7-alken-l-yl acetate 12, followed by the usual way to provide E-7-alken-1-ols 13.
Studies on the Chemical Composition of Essential Oil from Sap of Rhus Lac Tree
Du Yumin
1990, 11(6): 605-610.
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The chemical compositions of the essential oil of laccol and urushiol from the sap of Chinese lacquer tree are studied by GPCand GC-MS-DStechniques. The main components of these oils are 3-C
15
and 3-C
17
alkylcatechols, respectively, which were identified by their standard samples. The most abundant constituents are the monoenyl laccol and the trienyl urushiol. The other components are 4-C
15
alkylcatechols and 3-C
15
and C
17
alkylphenol. More than 98% of the commponents in essential oil were separated and identified by GC. The sap of lacquer tree contains 7%～9% of polymeric urushiol.
The Atomic Orbital Exponents and Orbital Electroncgativities of the Lanthanoid Elements in Different Electronic Configurations
Liu Guanghua, Ren Jingqing, Li Lemin, Xu Guangxian, Liang Zhenxuan
1990, 11(6): 611-616.
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The nonrclativistic Xa calculations were carried out in order to obtain the numerical atomic orbitals and orbital electronegativities of the lanthanoid ions in different electronic configurations. The single and double ζ exponents of Slater type basis functions of the atomic orbitals were then obtained by numerical fitting. The effect of charge and electronic configuration of the lanthanoid ions on the orbital exponent and electronegativity is studied and the regression formulas in higher precision are given. These fomulas not only show how the natures of the atomic orbitals vary with the ionic configuration but also provide the basic parameters for studies on the electronic structure of lanthanoid compounds and the iteration formulas for calculations through the self-consistence of charge approach.
A Study of Surface Acidity and Activity and Selectivity for Alkylation Benzene with Ethanol of HZSM-5 Modified Base-earth Metal Oxides
Pan Lurang, Li Hexuan
1990, 11(6): 617-621.
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The Surface acidities of HZSM-5 modified MgO, CaO, BaO were studied by means of TPD, IR, and the activity and the selectivity of alkylation benzene with ethanol to ethylbenzene were investigated. The results indicate that NH
3
desorption amount, 1550 cm
-1
(B-acid) on the IRspectra, activity and selectivity of alkylation decrease with increasing the content of oxide. Active sites of alkylation was discussed in this work.
Constructing Multicomponcnt Phase Diagram According to the Boundary Theory of Phase Diagram
Zhao Muyu, Wang Zhichen, Xiao Ping
1990, 11(6): 622-627.
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Applying our boundary theory of phase diagram, when the limited data are available, the multicomponent phase diagram can be constructed. H. Gupta constructed the multicomponent phase diagram by overlapping ZPF lines. By our method, it can be done more simply and directly, and the case which can not be treated by H. Gupta's method theoretically can be dealt with.
ESR Study of Benzene-Oxidation on V-P-O/SiO
2
Catalysts
Liu Jiageng, Ma Futai, Xu Yuanzhi
1990, 11(6): 628-632.
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The catalysts with the compositions (V
2
O
5
)
20
(P
2
O
5
)
x
(SiO
2
)
100
(0<x<60) were prepared by impregnation method. The catalytic properties of benzene oxidation on these samples were measured in a micro-reactor. The average oxidation numbers of V and the content of V
4+
were determined by potassium permaganate titration and ESR, respectively. Thus the contents of V
4+
and V
3+
were calculated and the results were related to the catalytic property. It is found that the conversion of benzene and the selectivity to MA in the reaction were related closely to the total content of V
5+
+ V
4+
and the content of V
4+
, respectively. By comparing the variation of the average oxidation numbers before and after reaction, we have come to the conclusion that the first attack to the aromatic ring is made by the lattice oxygen (double-boned).
A Study on Inhibition of Some Hetcrocyclic Compounds Containing Nitrogen for Corrosion of Mild Steel
Yang Baohe, Zou Jinyun, Kuang Fugui, Yao Luan
1990, 11(6): 633-637.
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It is investigated that the inhibition of pyridine, quinoline and their derivatives for the corrosion of mild steel in 1 mol/L HCl solution by weight-loss, impedance and polarization techniques. It is found that these compounds can inhibit both cathodic and anodic processes of mild steel. The corrosion potential shifts to less noble direction. The inhibition efficiency obtained by weight-loss is in good agreement with that obtained by impedance method. According to the relationship of the degree of coverage of pyridine or quinoline to its bulk concentration and system temperature, the adsorption of both inhibitors on mild steel follows Flory-Huggins isotherm. Thus, the thermodynamic parameters of the adsorption of pyridine and quinoline are evaluated from the adsorption isotherm. A possible adsorption modle of pyridine, quinoline and their derivatives on the surface of mild steel is also proposed.
Preparation and Its Catalytic Hydrogenation Behaviour of Silica Gel-Supported Polyvinylpyridine-Palladium Catalysts
Yang Shiyong, Sun Juntan, Li Hong, He Binglin
1990, 11(6): 638-642.
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Some basic polymers, such as poly-4-vinylpyridine and poly-2-vinylpyridine, were adsorbed on the surface of silica gel with the aid of the weak acidity of silica. The supported polymers were then complexed with PdCl
2
and reduced with NaBH
4
, the title catalysts were synthesized. The structures of the catalysts were characterized by XPS, UV/Vis, scanning and transmission electron microscope etc. The influence of preparation conditions and composition of the catalysts on the catalytic activity, stability and life period was examined. The catalysts synthesized possess a high catalytic activity for the hydrogenation of methylacrylate.
Catalytic Synthesis of Aspartame by Immobilized Thcrmolysin
Tao Guoliang, Chen Zhenhua, Zhuo Renxi
1990, 11(6): 643-646.
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In this paper, immobilized thermolysin was prepared by using aminopropyltriethoxysilane treated porous silica beads as carrier, and glutaraldehyde as crosslinking agent. The precursor of aspar-tame was synthesized in aqueous medium in good yield by the catalysis of the immobilized thermolysin, and aspartame was then obtained by the catalytic hydrogenolysis of the precursor. In the immobilized thermolysin-catalysed coupling reaction, the factors which affect the yield such as reaction time, temperature, medium pH, amount of the immobilized enzyme, substrate concentration and substrate molar ratio as well as concentration of calcium acetate were studied. Reuse of the immobilized thermolysin was also investigated.
Crystallization and Melting Behavior of PC/PET/EPDM Blend System
Li Ming, Ma Rongtang, Kou Xichun, Tang Xinyi
1990, 11(6): 647-651.
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The crystallization rate, crystallinity, Avrami exponent and melting temperature of the blend system of PC with PETand EPDM were investigated by means of depolarized light and differential scanning calorimetry respectively. Both of the crystallization rate and crystallinity of the blends of PET with PC, and with or without EPDM showed a marked drop with the increase of the content of PC. In contrast, the crystallization rate of blends of PET with EPDM was increased to a maximum when the weight fraction of EPDM was about 5%, but the crystallinity showed little change when the amount of addition of EPDM was up to 10%. The Avrami exponent, calculated on the basis of Avrami equation, did not seems to be influenced by the composition of blends. The DSC thermograms of annealed samples showed double melting peaks. The melting peak at higher temperature, i. e. melting point, shifted to the side of higher temperature with increasing PC content slightly and the melting peak at lower temperature shifted to the side of higher temperature when the annealing temperature was raised or the annealing time was prolonged.
The Improvement of Catalyst of Synthesizing Methacrylic Acid by One-step Oxidation of Isobutylaldchyde
Wu Tonghao, Yu Jianfeng, Yang Hongmao, Wang Goujia, Jiang Yuzi, Chi Hongpan, Zhang Xianjun, Sun Jinghui, Zhou Jianping
1990, 11(6): 652-653.
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Vibration frequency of the bridge oxygen of heteropoly molybdophosphoric acid has an obvious impact on the oxygen-insertion reaction. In order to improve its catalytic activity, the substitution of As for Pin the catalyst was tried. The results show that the catalyst with compositions P
1.13
As
0.2
· Mo
12
V
0.25
Sb
0.25
Cu
0.25
K
1.5
O
x
has a higher catalytic activity and that a better stability last 600 hours ex-perimentally. The yields of methacrylic acid and methacrolein are 71% and 11. 5% in single-pass reaction, respectively, and the conversion of isobutylaldehylde is 100%. Compared with the results obtained before, the yield of methacrylic acid was raised.
The Determination of Binary Heavy Rare Earth Mixture by Proportional Equation Method
Xu Liang, Gu Zhicheng
1990, 11(6): 654-656.
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When a binary mixture was determined with the proportional equation method according to the difference of reaction rates, the two equations could be set up by selecting two special times. t=0 and t→∞, if the reaction is reversible. Because of the initial concentration and the equilibrium concentration are independent of the reaction rate, the strict control of time in the experiment is unnecessary and a good result could be obtained. Based on this principle, the possibility of determining the binary heavy rare earth mixture by means of the ligand exchange reaction between RE arsenazo Ⅲ and CyDTA is discussed. Experimental results show that the relative error is less than 5% when the mixture of Dy and Er is in the range of 1 : 5～5 : 1 at 10～100 μg/25 mL level.
Syntheses and Studies of Properties on Potassium Salts of Heteropoly Acid of Bis-(9-W-2-MoP) with Lanthanoids
Zhao Benliang, Liu Jingfu, Zhu Zhiping
1990, 11(6): 657-659.
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The potassium salts of heteropoly acid with lanthanoids K
11
Ln(PMo
2
W
9
O
39
)
2
·nH
2
O, are prepared and thier elemental compositions are analysed. We entered into details on the stabilities to acid and base in aqueous solution and thermal stabilities of these compounds and determined thier IR spectra, UVspectra, XPS and
31
P NMR.
Crystal Structure of the Complex of Protonated 24-Mcmbcred Hexaaza-dioxa Macrocycle LH
4
+4
with Hcxaisothiocyanatocobalt(Ⅱ)
Jiang Zonghui, Wang Genglin, Yao Xinkan, Wang Honggen, Wang Ruji
1990, 11(6): 660-662.
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Anew complex of protonated 24-membered hexaaza-dioxa macrocycle LH
4
4+
with hex-aisothiocyanatocobalt( Ⅱ ) was synthesized and the crystal structure of [C
16
H
42
N
6
O
2
][Co(NCS)
6
] · Co (NO
3
)
2
· 4H
2
O was determined. It crystallizes in the triclinic system, space group P1(a = 7. 992(1)Å, 6=11. 007(2)Å, c-=27. 328(2)Å, a = 79. 01(2)°, β=81. 57(2)°, γ= 68. 70(2)°, V = 2190. 9Å
3
, Z=2). The protonated macrocycle L in the complex is in a boat type conformation. Comparing IR and NMR of the free protonated macrocycle L with those of the macrocycle L in the complex, it is proved that the conformation of the free protonated macrocycle L is the same as that of the macrocycle Lin the complex. The results obtained provide a basis for study of catalytic mechanism in supermolecule.The six-coordinated isothiocyanatocobalt complex anion [Co(NCS)
6
]
-4
is rare in the literature. Its structure is octahedral.
The Research of Behaviour of Polymer Adsorbent GDX 101 Used as the Stationary Phase of HPLC
Liu Yu, Yu Shilin
1990, 11(6): 663-665.
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Small and uniform particles (5～15 um) of GDX 101 resins can be obtained by grinding with a colloid mill and elutriating with a home-made solvent elutriation device. The resin elutriated is packed into a column by a high pressure slurry packing technique. In order to know the column performance, the permeability coefficient and efficiency of the column are calculated. Some samples of alkylbenzene are separated. The results show that GDX 101 can be used in HPLC and its behaviour is similar to that of the ODS column.
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