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中文
Table of Content
24 November 1992, Volume 13 Issue 11
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Articles
Studies on Structural Characteristics of Deal uminated Y Zeolites Treated by Different Methods
HUANG Yao, ZHU Chong-Ye, LI Quan-Zhi, DAI Lin-Shen, XUE Zhi-Yuan
1992, 13(11): 1335-1339.
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The microstructure of four kinds of dealuminated Yzeolites (USY,SSY,US-SSY,DAY) were studied by
29
Si,
27
AlMAS NMR,XRD and IR.The cause of the formation of non-framework Si,Al and Si-OH nests and of difference of their amount were discussed according to the methods of dealumination.It is shown that the different methods of dealumination brings about the removing of different Si(nAl) units on the framework of zeolites.The results of XRD indicate that the relative crystallinity of 97% can be obtained when SSY was further treated by the high temperature steam to US-SSY.After dealumination,if the remains of micropore is more and the secondary mesopore is less,the relative crystallinity of sample is higher.Finally,it was also found that the framework aluminium of unit cell (N
Al
)
F
measured by
29
Si MAS NMR is less than that measured by XRD and IR,and the reason was also discussed.
Preparation of Mo-Ni-P Impregnating Solution and Its Interaction with γ-Al
2
O
3
Support
JIANG An-Ren, ZHANG Yi-Bing, WANG Zhi-Hong, YANG Jun, DENG Jing-Fa
1992, 13(11): 1340-1344.
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The impregnating solution of Mo-Ni-Pprepared by using MoO
3
·H
2
O, NiCO
3
, H
3
PO
4
without the impurities of Na
+
and NH
4
+
is better than that made from MoO
3
, 2NiO(OH)
2
·Ni/CO
3
and H
3
PO
4
and no precipitation is found for being kept for a long time. According to the results of amonia-dissolving and XRDexperiments, a solubility threshold of Mo or Ni component on the support is found and the Mo/Ni mole ratio is 0. 8:1 after ammonia-dissolving. Component Pcan suppress the interaction of the support with the compound of Mo and Ni on the surface of the support. The TPRresults reveal that the suppression of the reduction of NiOby component Pis reduced by the interaction of Pwith support, and the reduction temperature of MoO
3
can also be decreased by the inrteraction between the compound of Mo and support. In addition, a suitable load amount of Mo-Ni-Pimpregnating solution is given.
The Ihermal Decomposition Mechanism of Lanthanum Hydroxide Dihydrogen Diphthalate Monohydrate
SUN Ju-Tang, ZHANG Ke-Lu, ZHANG Ji-Min, QIN Zi-Bin, FENG Yi-Li
1992, 13(11): 1345-1348.
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The thermal decomposition of lanthanum hydroxide dihydrogen diphthalate monohy-drate, LaOH (C
8
H
5
O
4
)
2
·H
2
O, was studied by thermogravimetric analysis. The products of thermal decomposition at various stages were characterized by infrared spectrometry,gas chro-matography and mass spectrography.The thermal decomposition of LaOH(C
8
H
5
O
4
)
2
·H
2
Oproceeded in five stages. LaOH(C
3
H
5
O
4
)
2
·H
2
O-La
2
(C
3
H
4
O
2
)
3
-La
4
O(CO
3
)
3
(C
8
H
4
O
4
)
2
-La
2
O (CO
3
)
2
La
2
O
2
CO
3
-La
2
O
3
,The phthalic anhydride ami 9,10-anthraquinone were formed as the condensates of gas phase products during the first and second stages, respectively.
Synthesis and Crystal Structure of Cerium Thiocyanate Complex with Tetraethylene Glycol [Ce(C
8
H
18
O
5
)(NCS)
3
(H
2
O)]
NI Zhao-Ai, LIN Feng, XU Cheng
1992, 13(11): 1349-1351.
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The title complex has been synthesized.In this complex there is only one tetraethy-lene glycol that acts as a pentadentate ligand and forms a ring-like structure.The excess coordination sites are satisfied by three thiocyanate ions and one water molecule.The coordination number of cerium is 9.The crystal structure of this complex was determined as follows:P1 space group with a=0.8816(3)nm,b=1.0465(2)nm,c=1.2490(2)nm,α=86.46(1)°,β=70.90(2)°,γ=66.37(2)°,V=0.9943 nm
3
,Z=2.The final deviation factor R=0.049,for 3497 unique reflections[I≥3°(I
0
)]
Studies on Reaction of Heteropolytungstoarsenate Anions [KAs
4
W
40
O
140
(M·H
2
O)
2
]
n-
in Organic Solvent
LIU Jing-Fu, GUO jun, LI Jin-Chang, ZHAO Ren-Liang, XU Gui-Ying
1992, 13(11): 1352-1354.
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The reaction of[KAs
4
W
10
O
140
(M·H
2
O)]
n-
(M=Mn
2+
,Co
2+
,Ni
2+
,Cu
2+
or Cr
2+
)anions in toluene is reported.The coordinated water molecules of the title anions can not be substituted by SCN
-
,Py in aqueous solution.However,she same replacement reaction takes easily in toluene.Some of the title anions can lose the coordinated water molecules directly leading to coordmatively unsaturated site on the surface of the anions in toluene.Synthesis and oxidation properly of the high oxidation state complexes are also reported.
Crystal Structure of Nickel(Ⅱ) Complex with Mono-Schiff Bases from Picolinaldehyde N-Oxide and 1,2-Propanediamine
YAN Shi-Ping, JIANG Zong-Hui, LIAO Dai-Zheng, WANG Geng-Lin, WANG Ru-Ji, WANG Hong-Gen, YAO Xin-Kan
1992, 13(11): 1355-1357.
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The crystal structure of nickel(Ⅱ)complex of mono-schiff bases from picolinaldehyde N-oxide and 1,2-propanediamine was determined by X-ray diffraction.The crystal belongs to monoclinic system,space group P2
1
/c,a=0.8199(1)nm,b=3.364(3)nm,c=0.9325(2)nm,β=97.32(2)°,V=2.551 nm
3
,M=616.04,Z=4,D
x
=1.57 g/cm
3
,μ=10.33 cm
-1
,F(000)=1272,R=0.068.The coordination number of Ni(Ⅱ)is six.Ni(Ⅱ)ion in the complex is in octahedral environment of coordination.
Synthesis of Zeolites from Non-alkaline Media
ZHAO Da-Qing, QIU Shi-Lun, DING Hong, PANG Wen-Qin
1992, 13(11): 1358-1360.
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Zeolite P,ZSM-39,Theta-1 and ZSM-5 were synthesized by hydrothermal crystallization from non-alkaline media in the presence of fluoride ions by using various organic templates,and characterized by means of thermal analysis and scanning electron microscopy technique.Large single crystals of zeolite P,ZSM-39 and ZSM-5 were obtained.The influence of compositions of starting mixtures and temperature on the zeolite synthesis was investigated.
Syntheses and Characterization of Heterotrimetalophosphates
WANG Jin-Xi, YANG Shu, YANG YU-Xiang, LIU Hai-Cheng, CHEN Rong-San
1992, 13(11): 1361-1363.
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Three new heterotrimetalophosphatesα-[(C
4
H
9
)
4
N]
4
[PW
9
Mo
2
VO
10
],α-[(C
4
H
9
)
4
N]
4
[H
2
PW
9
Mo
2
AlO
10
] and α-[(C
4
H
9
)
4
N]
4
[H
2
PW
9
Mo
2
FeO
40
]were synthesized.The compounds were determined and characterized by elementary analysis,UV,IR,DTA-TG and CV.
A Study on Determination of Sulfide and Sulfite By Microwave Induced Plasma Atomic Emission Spectrometry with Gas Generation for Sample Introduction
ZHANG Jin-Sheng, ZHANG Han-Qi, DUAN Yi-Xiang, XU Fang, JIN Qin-Han, WANG Da-Ning, ZOU Ming-Qiang, LIU Li
1992, 13(11): 1364-1367.
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In this paper,the determination of S
2-
and SO
3
2-
in solution were investigated by gas generation MIPAES.In the reaction cell S
2-
and SO
3
2-
reacted chemically with H
2
SO
4
and formed H
2
S and SO
2
,respectively.The H
2
S and SO
2
generated were carried into the MIP and the emission intensity at 216.9 nm was recorded.Various experimental conditions for determining S
2-
and SO
3
2-
were studied.The detection limits for S
2-
and SO
3
2-
are 0.08μg and 0.25μg.respectively.Good precision(RSD<5%)were observed either for S
2-
or for SO
3
2-
.
Studies on the Mechanism of Coordination Reaction of Porphyrins with Some Metal Ions by Fluorometry
LI Jia, PAN Zu-Ting, XU Mian-Yi
1992, 13(11): 1368-1370.
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The present paper covers the mechanism of coordination reaction of porphyrins with some metal ions studied by fluorometry and the catalytic mechanism of some catalysts.Three kinds of porphyrins were tetrakis-(4-trimethylammoniumphenyl)porphyrin(TAPP),tetrakis-(4-sulphophenyl)porphyrin(TPPS
4
)and tetrakis-(4-pyridyl)porphyrin(TPyP),The general conditions of the coordination reaction of porphyrins with metal ions were explained and concluded successfully.
Studies on the Charge-Transfer Complexes of Amino Acids with Chloranil by Spectrophotometry
TONG Shen-Yang, LI Na
1992, 13(11): 1371-1373.
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The charge-transfer complexes of chloranil with five amino acids,Glycine,L-leucine,L-lysine,L-serine and L-cystine,were studied in detail by spectrophotometry.Anew and single method for the determination of amino acids has been established.The determinations was carried out in the solution of 20%(V%)ethanol with pH 9 at 350 nm.The equilibrium constants were determined.The composition of the charge-transfer complexes was also discussed.
Investigation on Carbon Fiber Microelectrode(Ⅺ)——The Determination of the Thermodynamic and Kinetic Parameters by the Temperature Effect
JU Huang-Xian, CHEN Hong-Yuan, GAO Hong(H. Kao)
1992, 13(11): 1374-1377.
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The effects of temperature on the electrochemical behaviour of ferrocene and its derivative at a carbon fiber microelectrode were studied.By means of the noble feature of micro-electrode,and the temperature effect on currents,electrode potentials as well as heterogeneous electron transfer rate constant,a number of thermodynamic and kinetic parameters,such as E
al
,D
0
,k",ΔS",ΔG",ΔH",Q′
H
and K,were determined.
Fluorimetric Studies on Complexes of Tetracycline Antibiotics Degradation Products with Alkaline Earth Metals
ZHAO Yi-Bing, CHANG Wen-Bao, CI Yun-Xiang
1992, 13(11): 1378-1379.
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This paper first describes the sensitive detections of tetracycline antibiotics,which are propertional to the fluorescent intensities of complexes of their alkaline degradation products with alkaline earth metals.The structures of the complexes and the interferences of coexisting ions are discussed.This method are useful in clinical assay and diagnosis.
Determination of Caffeine by Differential Pulse Voltammetry with Nafion Coating Carbon Fibre Electrode
SUN Chang-Qing, CAO Qian, XU Hong-Ding, GUO Li-Ping
1992, 13(11): 1380-1382.
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A Nafion modified carbon fibre microelectrode was established.The response of caffeine at the Nafion coating microelectrode was evaluated by differential pulse voltammetry.The linear relationship between the peak height and the concentration of caffeine in the range of 2×10
-5
～5×10
-4
mol/Lis obtained.By means of cyclic voltammetry the kinetic behaviour of caffeine on the electrode was studied.This method was also applied to the direct determination of caffeine in drugs.
Measurement of the Overall Separation Degree of Thin Layer Chromatography
GE Zao-Chuan, LIN Hui-Gai
1992, 13(11): 1383-1385.
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Based on the resolution in chromatography,a new degree of separation of thin layer chromatography was developed for measuring the overall separation degree of multicomponent chromatogram.The degree of separation was used as the optimization criterion of experimental condition optimization and satisfactory results were obtained.
Laser Opto-thermal On-line Detection for the Gel Capillary Electrophoresis
DENG Yan-Zhuo, YU Pei, YE Meng-Wei, LIU Heng-Biao
1992, 13(11): 1386-1388.
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The opto-thermal detection technique based on crossed-beam thermal lens effect has been developed for the on-line determination of capillary polyacrylamide gel electrophoresis(PAGE).The minimum detectable concentration of methylene blue in ethanol filled into 220 pm i.d.capillary was obtained to be 1.76×10
-9
mol/L,corresponding to the absorbance of 3.8×10
-6
.Amixture of bromophenol blue and amide black was separated by capillary PAGE and detected by laser opto-thermal on-line detection technique.Mass detection limit for bromophenol blue injected into the gel capillary was found to be 40 pg.
The Conformation of Cyclododecene
XUE Jie-You, LU Xiang-Jun, LAI Cheng-Ming, LIN Shao-Fan, TANG Shi-Xiong, WANG Xiao-Lan
1992, 13(11): 1389-1393.
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The structure parameters of 15-phenyl bicyclo[10,3,0]pentadec-l(12)-en-13-one with [1
ene
2333] conformation of the cyclododecene moiety calculated by molecular mechanics method(MMX program)are in good agreement with the experimental data of X-ray diffraction.Based on the steric energy of fifteen possible conformations of the cis-cyclododecene,the [l
ene
The Crystal Structure and Conformation of trans-1,2-Bis[5-(2,5-dimethyIphenyl )oxazol-2-yl]cyclopropane
XUE Jie-You, ZHANG Wen-Qin, WANG Ming-Zhen, LI Hui-Jie, GAO Zhen-Heng, LU Xiang-Jun, WANG Hong-Gen, LIN Shao-Fan
1992, 13(11): 1394-1397.
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Trans-1,2-bis[5-(2,5-dimethylphenyl)oxazol-2-yl]cyclopropane was synthesized and its crystal structure was determined by X-ray crystallographic method.The crystal is monoclinic,space group P2
1
/c with unit cell dimentions a=1.3465(2)nm,b=0.8021(1)nm,c=l.9277(37)nm;β=105.99(1)°V=2.001(1)nm
3
and Z=4.The calculation of molecular mechanics force field(MMS program)provided the structure and conformation of the title compound,which are in good agreement with the results from X-ray determination.The oxazole rings and cyclopropane ring are arranged in a stable gauche conformation with the dihedral angles of 86.04° and 73.26°,which leads to a better conjugation between them.Besides,the relationship between the conformation and UV spectra of POCOP system is discussed.
Synthesis and Conductivity of Organometallic Solids [Fe(CpMe)
2
][M(dmit)
2
] and [FeCp(Tol)]n[M(dmit)
2
]
QIN Jin-Gui, ZHOU Wei-Hua, DING Yong-Pmg, LIU Dao-Yu
1992, 13(11): 1398-1400.
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Six new organometallic radical ionic salts,[Fe(CpMe)
2
][M(dmit)
2
] and [FeCp(Tol)]
n
[M(dmit)
2
]
n
(M=Ni,Pd,Pt,Cu or Co;CpMe=methylcyclopentadienyl;Tol=toluene;H
2
dmit=4,5-dimercapto-1,3-dithiole-2-thione;n=1 or 2)were synthesized,and characterized by elemental analysis,infrared and mass spectroscopy.The electrical conductivity of solid state was reported and discussed in terms of structure-property relationship.
Synthesis and Structure Analysis of Ti-Mo Heterobimetallic Complexes
WANG Ji-Tao, ZHANG Yun-Wen, XU Yu-Ming, ZHOU Ren-Jie
1992, 13(11): 1401-1405.
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Thirteen Ti-Mo heterobimetallic complexes were prepared.The structures of these complexes were characterized by element analysis,
1
H NMR,
13
C NMR,
95
Mo NMR,
11
B NMR,IR,MS and electrical conductivity.The heterobimetallic complexes contain metal-metal bonds with some covalent character and semibridging carbon monoxide.The common structural formula of Ti-Mo heterobi metallic complexes can be written as follow: Where R=H,Pz;X=H,CH
3
;Y=H,CH
3
,R=CH
3
,OCH
3
,OC
2
H
5
.
Studies on Chiral Thiophosphoric Acids and Their Derivatives(Ⅸ)----Stereochemistry of Hydrolysis of O-Ethyl O-Phenyl Thiophosphoramides
TANG Chu-Chi, ZHANG Mian-Ji, ZHANG Dian-Kun
1992, 13(11): 1406-1410.
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The reaction of optically active(+)-(S)-Oethyl O-phenyl thiophosphorochloride with various primary or secondary amines in the presence of base gave the optically active(-)-or(+)-(S)-O-ethyl O-Phenyl N,N,-dialkyl(or N-alkyl)thiophosphoramides 2 with the inversion of configuration at phosphorus atom.The acid hydrolysis of 2 was carried out in 6 mol/Lor 9 mol/L HCl/dioxane solution,and resulted in the cleavage of P-N bond,giving the products with the inversion of configuration.The alkaline hydrolysis of 2 occurred in 1 mol/Lor 3 mol/L NaOH/dioxane solution,and gave the products with the inversion of configuration with PhOas the leaving group.These hydrolysis mechanisms can be satisfactorily explained in the light of trigonal bipyramidal(TBP)intermediates concept.
Sytheses, Structure and SAR Study on New Sulfonylurea Compounds(Ⅰ)——Crystal and Molecular Structure of N-(2'-pyrimidinyl)-2-ethyl Carboxylate-benzene Sulfonyl urea
LI Zheng-Ming, JIA Guo-Feng, WANG Ling-Xiu, LAI Cheng-Ming, WANG Ru-Ji, WANG Hong-Gen
1992, 13(11): 1411-1414.
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Synthesis and crystal structure of title molecule was reported here.The crystal is monoclinic,belonging to space group P2
1
/a with unit cell parameter a=0.7384(2)nm,b=2.1496(4)nm,c=0.9973(2)nm,β=90.12(2)°,V=1.576 nm
3
,Z=4,R=0.059 for 1421 reflections.Molecular structure was discussed.There are three different planes in molecule,in each of which a conjugated system was formed.The empty 3
dxz
orbital of atom Senters the formation of conjugated bond.The intra-molecule hydrogen bond between atom Nand Hwas found.
Micellar Bis-quaternary Ammonium Salts Containing Oxaethylene Chain Catalytic Abnormal Reimer-Tiemann Reaction
CHEN Ji-Jun, DU Zheng-Ming, SHI Yao-Zeng, SONG Tao, HU Hong-Wen
1992, 13(11): 1415-1417.
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The micellar and non-micellar bis-quaternary ammonium salts containing oxaethylene chain,DMOU I,BTMOU CLand BTMU CL,were synthesized and their catalytic activity were compared in the abnormal Reimer-Tiemann reaction.The micelle was better than the non-micelle.
A New Diterpenoid Alkaloid from
Delphinium Caeruleum
PAN Yuan-Jiang, WANG Rui, CHEN Shao-Nong, CHEN Yao-Zu
1992, 13(11): 1418-1419.
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A new minor diterpenoid alkaloid,caeruline(1),was isolated from Delphinium,caeruleum Jacq.ex Camb.Its structure was elucidated on the basis of spectral analysis.Along with this new compound,three known diterpenoid alkaloids(tatsiensine,delcosine and lycocto-nine)were also isolated.They have not been isolated in this plant previously.
Electrochemical Behaviour of Cyanoethenyl Aniline Derivatives
ZHANG Dong, JIANG Yue-Shun, WANG De-Jun, YANG Sai-Peng, LI Tie-Jin, ZHANG Bao-Wen
1992, 13(11): 1420-1423.
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The electrochemical behaviour of the electron donor-acceptor model compounds,cya-noethenyl aniline derivatives was investigated by cyclic voltammetry.The effects of donating electron group-NH
2
,-N(CH
3
)
2
and withdrawing electron group cyanothenyl group on electrochemical behaviour of these compounds were studied in detail.The structures of electroox-idation and electroreduction state of these compounds were proposed,and the mechanism of the electrode reaction was studied by comparing the effects of tert-radical,sec-radical and pri-radical on electrochemical behaviour of these compounds.
The Kinetics of Emulsifier-Free Emulsion Polymerization of Styrene-Butyl Acrylate and TEM Analysis
DAI Li-Zong, ZOU You-Si, PAN Rong-Hua
1992, 13(11): 1424-1427.
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The influence of temperature on pHof system of emulsifier-free emulsion polymerization of styrene-butyl acrylate in the presence of sodium undecylenate is discussed.The curve of polymerization kinetics is described.The reaction rate constant(k
P
)at different temperatures is calculated.Using TEMto compare emulsion polymerization of several emulsifier system,we found that the homogeneity and adhesion and deformation of the particles of emulsion could be controlled.Because there are no free emulsifier,the stability of emulsion is raised.
Synthesis and Properties of Triheteropoly Compounds Containing Mn,Co,Ni
WANG Jun, WU Zhi-Yun, ZHANG Heng-Bin, ZHAO Zhong-Qing, WANG Xian-Ren, WEI Quan
1992, 13(11): 1428-1431.
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Five heteropoly silicotungstic compunds were synthesized.Their properties were characterized.The results indicate that the IRabsorption of W-O
c
-W and Si-O bonds,the electronic bonding energy of constituent elements,the reducibility of W-Opolyhedra,the lattice size and crystal shape of heteropoly compound and the thermal stability of Keggin unit etc.are changed obviously,when Watom in Keggin anion was substituted for a alcunary or a lower valence transition metal ion such as Mn
2+
,Co
2+
and Ni
2+
.In the paper,the correlation of the properties of the transition metals with the changes mentioned above was discussed.
Infrared and Raman Spectra of Tetra(
p
-nitrophenyl) Porphyrin and Its Transition Metal Complexes
SHI Tong-Shun, ZHENG Guo-Dong, ZHOU Jian-Gang, LI Dong-Mei, CAO Xi-Zhang, DONG Qing-Rong
1992, 13(11): 1432-1435.
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The Infrared spectra(220-3500 cm
-1
)and Raman spectra(100-1700 cm
-1
)of te-tra(p-nitrophenyl)porphyrin and its Cr(Ⅲ),Mn(Ⅲ),Fe(Ⅲ),Co(Ⅱ),Ni(Ⅱ),Cu(Ⅱ)and Zn(Ⅱ)complexes were measured and investigated respectively.The band at 3321 cm
-1
and 988 cm
-1
belonging to N-Hvibrations of pyrrole disappears when the complex formed.The metal sensitive bands were found at ～1600,～1582,～1547,～1284,～1190,～355 and ～245 cm
-1
.The bands at
3
55 and
2
45 cm
-1
of the complexes decrease in wave number in the order of Ni(Ⅱ)>Co(Ⅱ)>Cu(Ⅱ)>Zn(Ⅱ).The bands at ～3110,～1600,～1520,～1350,～850 and ～825 cm
-1
resulted from p-nitrobenzene of the porphyrin.
The Influences of Isomer Structures of Polyacetylene on the Stability and Electronic Properties of Polyacetylene Sulfide
SU Zhong-Min, FU Yu-Jie, WANG Rong-Shun
1992, 13(11): 1436-1439.
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In this paper,the influences of isomer structures of polyacetylene on the stability and electronic properties of polyacetylene sulfide were discussed by means of the tight-binding LCAO-SCF-MO method.The reasons for the influence were revealed.The calculation indicated that the trans-PAis the stablest structure in energy,sulfidation made it furtherly stable.
Studies on Thermokinetics (XXIV)——Thermokinetics Method for the Third Order Reaction
WANG Rui-Lin, DUAN Zhi-Hua, ZENG Xian-Cheng, QIN Zi-ming, DENG Yu
1992, 13(11): 1440-1443.
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On the theoretical basis of thermokinetics proposed in the literature,the method of di-mensionless parameters for the third order reactions are derived in this paper.This method has been used to study the formation of hexamethylenetetramine in aqueous solutions at two different temperatures.The rate constants of these reactions calculated by using this method are in agreement with the values in literature.And therefore,the foundamental equations of thermokinetic method for the third order reactions are believed to be correct.
The Determination of Dismutation Rate Constant of Superoxide Ion Catalyzed by SOD Model Compound with Tast Polarography
JIANG Yi-Qin, LIU Wan-Qiao, TANG Kai-Qing, LIAO Zhan-Ru, CHEN Pei-Ling, SHI Ju-En
1992, 13(11): 1444-1447.
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The SOD model compound-catalyzed dismutation reaction of superoxide ion O
2
-
in aprotic solvent has been studied by tast polarography.Asimplified function is made to replace the exact solution of the kinetic differential equantion with error less than 1%.The catalytic dismutation rate constant k
1
is determined by the measurement of the ratio between the catalytic and diffusional current as a function of SOD model compound concentration and the drop time of dropping mercury electrode.
EPR Study on Correlation Between aN Values of Trifluoromethyl
t
-Butyl Nitroxide and Solvent Parameters
E
T
and
Z
(kosower)
ZHAO Cheng-Xue, PENG Yi-Yuan, QU YAN-Ling, PENG Hong
1992, 13(11): 1448-1451.
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Trifluoromethyl t-Butyl nitroxide generated in the electron transfer reaction between(CF
3
CO
2
)
2
and t-BuNHOCOPh was subjected to EPRstudy in
16
solvents with different polarities.The result shows the linear relationships as aN=(2.17×10
-2
ET +11.34)×10
-4
T(r=0.975)and a
N
=(1.20×10
-2
Z+11.46)×10
-4
T(r=0.976).By making use of such a fluori-nated un-bulky nitroxide as the model molecule,much information of theoretical importance about the solvation as well as the electronic structure of the nitroxide have been disclosed.
Studies on Electronic Structures and Spectra of Heteroatom-Substituted Porphyrins
YANG Ming, WANG Zhi-Zhong, YANG Zhong-Zhi
1992, 13(11): 1452-1456.
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Systematical calculation studies on the electronic structures and singlet π→π
*
transitions of free porphyrins and oxa-,thia-or aza-porphyrins have been made by using INDO/CImethod.Based on the frontier orbital characters and charge distributions the electronic structures of these compounds are discussed.The calculational results predict the spectra of lower energy transition of some heteroatom-substituted porphyrins.
Computation of Auxiliary Functions in Molecular Integrals up to Arbitrary Accuracy(Ⅲ)——Optimization of Backword Recursive Algorithm of Incomplete Gamma Function F
m
(x)
Li Yan-Xin, Dong Xia-Lan, Pan Shou-Fu
1992, 13(11): 1457-1461.
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Strict error analysis is carried out for two kinds of backward recursive algorithm,series expansion and continued fraction approximation,of incomplete Gamma function F
m
(x).We obtain the conditions of numerical stability for both algorithms and further suggest an optimal strategy with discussions.
Preparation and Synthesis of Hydrotalc in Microwave Field
HE He-Ming, JIANG Da-Zhen, SUN Tie
1992, 13(11): 1462-1463.
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The present study reports the synthesis of hydrotalc and hydrotalc-like substance by microwave method,which was compared with that of the conventional hydrothermal method.The microwave method gave a good quality product rapidly.By the characterization of XRD and IR,it was found that the hydrotalc can be intercalated easily and exchanged completely with anions.The intercalating products possess a long-range order.
Studies on Catalyst of Oxidation of
t
-Butanol to MAA and MAL
WANG Guo-Jia, WU Tong-Hao, YANG Hong-Mao, JIANG Yu-Zi
1992, 13(11): 1464-1465.
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A seven-element oxide catalyst system with a high activity,selectivity and stabilitywas studied.The yields of MAA + MAL are 83.2%,and the conversion of t-BuOH is 100% when Mo
12
Co
8
Fe
4
Bi
4
Ni
4
Te
0.7
K
0.04
was used as the catalyst.The element play an important role in improving the catalytic activity and selectivity.If we use two step reactors,that is the first and second step reactor,contain the above catalyst and P
1.13
Mo
12
V
0.25
Cu
0.25
Sb
0.25
K
1.5
As
0.2
respectively,the yields of MAA and MAL are 63.2% and 6.5% respectively,and the conversion of t-BuOH is 100%.
Reduced Extent Method for Thermokinetics of
n
-Order Reactions
LIU Jing-Song, ZENG Xian-Cheng, DENG Yu
1992, 13(11): 1466-1468.
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A reduced extent method for thermokinetics of n-order reactions is proposed,which is used for calculating the rate constants and determining the orders of reactions.The applications of the method are given,whose results are in agreement with those in literatures.And therefore,the method for thermokinetics of n-order reactions is believed to be correct.
Synthesis and Characterization of Poly(
p
-Phenylphenoxyphosphazine)
ZHENG Fu-An, LIN Zhi-Hong, YIE Chun-Min, TANG Xin-Yi
1992, 13(11): 1469-1471.
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The solution polymerization method of poly(dichlorophosphazene)from hexachlorocy-clotriphosphazene with a-chloronaphthalene as solvent was investigated and the title polymer was prepared from polydichlorophosphazene and sodium p-pheny|phenolate.At the same time,the IR,
1
H NMR of the title polymer were determined.The M
n
of this polymer estimated by GPC is 6×10
4
and the glass transition and viscous flow temperatures determinated by TBAare 0℃ and 130℃ respectively.
Studies on Immobilization of β-Cyclodextrin onto Polymeric Carrier (Ⅱ)
HE Bing-Lin, ZHAO Xiao-Bin
1992, 13(11): 1472-1475.
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A novel β-cyclodextrin polymer was prepared by immobilization of β-cyclodextrin onto chlorosulfonated and crosslinked polystyrene carrier via chemically bonding.Experimental results show that the β-cyclodextrin polymers made by the two systems of NaH/DMFand Et
3
N/ DMAP/DMF have high immobilization amounts.The influence factors were studied in detail.
Studies on Gelation Kinetics of Pol yacrylamide
WANG Guang-Xin, CHEN Zhong-Qi, YANG Xin-Dong, CHEN Li-Dian
1992, 13(11): 1476-1478.
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In this research work,kinetic behaviour of polyacrylamide(PA)aqueous solution in the presence of Cr(Ⅲ) during the gelation process were investigated quantitatively.Experiments revealed that the gelation process of PAwith Cr(Ⅲ) might be divided into three stages:accelera-tive,steady state and final stages.The increase rate of viscosity of the system represents the formation rate of the gel net.And the apparent rate constants and apparent activation energy in the steady-state stage of gelation were measured.
Behavior of Ethylene-Propylene Copolymerization over Supported Titanium Catalyst
WU Qing, LIN Shang-An
1992, 13(11): 1479-1481.
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The time dependence of ethylene-propylene copolymerization rate over TiCl
4
/MgCl
2
/ EB-AlEt
3
catalyst was studied.An enhanced rate of ethylene polymerization after brief copolymerization with propylene,which is much faster in comparison with that of conventional ethylene polymerization,and decaying-type kinetics were shown.It was found that the copolymerization brings about a change of morphology of the catalyst-polymer particles to loose structure.This allows the monomers diffusing more easily and developing potential activity of the catalyst,resulting in higher polymerization rate and different kinetic behavior from the homopolymerization.
Studies on Slow Release of the Core Material and Function of the Capsule Containing P204
ZHANG He-Zhe, WANG Yu-Jie, BAI Guang-Yue, YAN Zhang, LIU Shu-Hua
1992, 13(11): 1482-1484.
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We measured the permeable efficiencies of KCl through the polyamine capsule with core material KCl.If the capsules were soaked in bis-(2-ethyl-hexyl)phosphate(P204),the permeable efficiency was reduced obviously.Therefore,we may change the permeability of the core material.The permeable efficiency of KCl was increased in electric field.Moreover,the ON and OFF of electric field can result in the change of permeable velocity of KCl,and it has the better function of reversable permeation.
Preparation of Polymeric Microparticles by Improved Microsuspension Polymerization
ZHANG Yu-Ge, WANG Bu-Sen, CHEN Hong-Bin, NING Jun, HE Bing-Lin
1992, 13(11): 1485-1487.
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The present paper represents the improved microsuspension polymerization for the preparation of polymeric microparticles.The effects of several factors on the stability of the system were studied.The results show that it could be carried out in a wide range of reaction conditions.The method may be applied to batch production of polymeric microparticles.
Preparative Studies on Monodisperesed Polymeric Microparticles and High Efficiency Stationary Phase for Anion Chromatography
CHEN Hong-Bin, ZHANG Yu-Ge, WANG Bu-Sen, HE Bing-Lin, NING Jun
1992, 13(11): 1488-1490.
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Monodispersed polymeric microparticles were prepared by seed-polymerization.The anion chromatographic stationary phase packings were obtained by coating the surface-sulfonated particles with quarternarized latexes.This packing is of high efficiency and excellent duplicate properties for common inorganic anions.
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