1986 Volume 3 Issue 1
1986, 3(1): 1-8
Abstract:
This paper reviewed some new progresses of the metathesis reaction of functionalized olefins including unsaturated esters, ketones,ethers and unsaturated nitrogen and halogen containing compounds.
This paper reviewed some new progresses of the metathesis reaction of functionalized olefins including unsaturated esters, ketones,ethers and unsaturated nitrogen and halogen containing compounds.
1986, 3(1): 9-13
Abstract:
In this paper reaction of polyglycidylmethacrylate with α-amino acid is discussed.Through the reaction some polymer ligand resins grafted with various α-amino acids were obtained. L-Proline grafted on polyglycidylmethacrylate was able to be complexed with copper(Ⅱ) ions and it could be used for the complete resolution of D, L-phe by column chromatography, and D-enatiomer was eluated in front of the L-isomer.
In this paper reaction of polyglycidylmethacrylate with α-amino acid is discussed.Through the reaction some polymer ligand resins grafted with various α-amino acids were obtained. L-Proline grafted on polyglycidylmethacrylate was able to be complexed with copper(Ⅱ) ions and it could be used for the complete resolution of D, L-phe by column chromatography, and D-enatiomer was eluated in front of the L-isomer.
1986, 3(1): 14-18
Abstract:
The microgel in the fractions of cis-poly-isoprene polymerized by lanthanide catalyst was determined with the aid of Guinier plots of the light scattering data, and the monodisperse Mark-Houwink equation of the linear polyisoprene in the sol of the polymer was deduced.
The microgel in the fractions of cis-poly-isoprene polymerized by lanthanide catalyst was determined with the aid of Guinier plots of the light scattering data, and the monodisperse Mark-Houwink equation of the linear polyisoprene in the sol of the polymer was deduced.
1986, 3(1): 19-23
Abstract:
The oxidation of methane to formaldehyde on various Sn-Zr and Sn-Zr-Ce oxide catalysts have been investigated. The adsorption-desorption of n-butylamine and oxygen on the catalysts have been carried out by temperature programmed desorption method. The yield of formaldehyde was found to be correlative with Sn/Zr ratio and the amount of cerium in the catalysts. The activity of the catalyst in the formation of formaldehyde from methane was dependent upon the acidity of the catalyst and chemisorption states of oxygen. The results obtained from X-ray diffraction show that there is a strong influence of oxides of Sn in the catalyst on the activity.
The oxidation of methane to formaldehyde on various Sn-Zr and Sn-Zr-Ce oxide catalysts have been investigated. The adsorption-desorption of n-butylamine and oxygen on the catalysts have been carried out by temperature programmed desorption method. The yield of formaldehyde was found to be correlative with Sn/Zr ratio and the amount of cerium in the catalysts. The activity of the catalyst in the formation of formaldehyde from methane was dependent upon the acidity of the catalyst and chemisorption states of oxygen. The results obtained from X-ray diffraction show that there is a strong influence of oxides of Sn in the catalyst on the activity.
1986, 3(1): 24-29
Abstract:
Ring-shaped polystyrene (RPS) was prepared through cyclization reaction of linear polystyrene with active end groups. Systematical characterization of RPS fractions was carried out by GPC-low angle laser light scattering spectroscopy and other methods. The mean value of the ratio g(=[η]r/[η]1) is 0.63 in θ solvent and~0.65 in good solvents. The ratio of unperturbed mean square radius of gyration between ring and linear polystyrene (1>or/2>ol) is 0.55-0.59. They are both coincide with theoretical values for macro rings. It is found that RPS complys with universal calibration cuvve of GPC and has smaller hydrodynamic volume than linear polystyrene. Parameters of Mark-Houwink equations of RPS in cyclohexane 34.5℃,toluene 25℃ and tetrahydrofuran 30℃ have been obtained as K equals to 5.0, 0.683 and 1.2×10-2;α equals to 0.5, 0.734 and 0.68 respectively.
Ring-shaped polystyrene (RPS) was prepared through cyclization reaction of linear polystyrene with active end groups. Systematical characterization of RPS fractions was carried out by GPC-low angle laser light scattering spectroscopy and other methods. The mean value of the ratio g(=[η]r/[η]1) is 0.63 in θ solvent and~0.65 in good solvents. The ratio of unperturbed mean square radius of gyration between ring and linear polystyrene (
1986, 3(1): 30-35
Abstract:
25MHz Carbon-13 NMR spectra were used to study end group and branched structure of H2O2-initiated liquid hydroxy terminated polybutadiene (HTPB) obtained in ethanol.The carbon-13 spectra of the three main primary alcohols have been assigned. Recognition of RCH:CHCH2OH(Ⅰ) and RR C:CH2OH(Ⅱ) resonances strongly supports the structure Ⅰ and Ⅱ. The ethanol used as solvent in polymerization may be introduced into polymer, forming end group structure, dominantly RCH:CHCH2CH(OH)CH3 (cis and trans). Its hydroxy content was about 8% of total hydroxy amount in HTPB. Some terminal alcohol, aldehyde groups and branched structures have also been determined,but their contents were minor in HTPB.
25MHz Carbon-13 NMR spectra were used to study end group and branched structure of H2O2-initiated liquid hydroxy terminated polybutadiene (HTPB) obtained in ethanol.The carbon-13 spectra of the three main primary alcohols have been assigned. Recognition of RCH:CHCH2OH(Ⅰ) and RR C:CH2OH(Ⅱ) resonances strongly supports the structure Ⅰ and Ⅱ. The ethanol used as solvent in polymerization may be introduced into polymer, forming end group structure, dominantly RCH:CHCH2CH(OH)CH3 (cis and trans). Its hydroxy content was about 8% of total hydroxy amount in HTPB. Some terminal alcohol, aldehyde groups and branched structures have also been determined,but their contents were minor in HTPB.
1986, 3(1): 36-40
Abstract:
The catalytic behaviour of 12-molybdophospboric acid and its salts in the decomposition reaction of H2O2 has been studied by comparing them with the conventional Fenton reagent.The results showed that 12-molybdophosphoric acid gives only negligible catalytica ctivity, while its salts have the activity comparable to that of the Fenton reagent. It is suggested that the active species were metallic counterions from heteropolyacid salt. The activity of 12-molybdophosphoric acid was markedly affected by substitution of Mo+6 in the polyanion by V+5 and increased regularly with the number of V+5 substituted. For the decomposition reaction of H2O2 by 12-molybdophosphoric acid a S-shaped kinetic curvewas given rather than a parabolic one as in the case of Fenton reagent. The S-shaped curve is characteristic of branch chain reaction and indicates the formation of more active intermediate as a result of the reaction betwcen V+5 in the active center of polyanion and the substracte.
The catalytic behaviour of 12-molybdophospboric acid and its salts in the decomposition reaction of H2O2 has been studied by comparing them with the conventional Fenton reagent.The results showed that 12-molybdophosphoric acid gives only negligible catalytica ctivity, while its salts have the activity comparable to that of the Fenton reagent. It is suggested that the active species were metallic counterions from heteropolyacid salt. The activity of 12-molybdophosphoric acid was markedly affected by substitution of Mo+6 in the polyanion by V+5 and increased regularly with the number of V+5 substituted. For the decomposition reaction of H2O2 by 12-molybdophosphoric acid a S-shaped kinetic curvewas given rather than a parabolic one as in the case of Fenton reagent. The S-shaped curve is characteristic of branch chain reaction and indicates the formation of more active intermediate as a result of the reaction betwcen V+5 in the active center of polyanion and the substracte.
1986, 3(1): 41-45
Abstract:
The glass transition temperature of regular star-shaped block copolymers of polystyrene and polyisoprene with different arm length and branch degree are measured by linear dilatometer and dynamic Rheovibron Viscoelastometer. The values of TgI and Tg(S) depend on the morphology, branch degree and the arm length of these polymers. The effect of these factors on the glass transition temperature of dispersed phase, TgS), is found to be more noteworthy. The intermediate phase relaxation is suggested.
The glass transition temperature of regular star-shaped block copolymers of polystyrene and polyisoprene with different arm length and branch degree are measured by linear dilatometer and dynamic Rheovibron Viscoelastometer. The values of TgI and Tg(S) depend on the morphology, branch degree and the arm length of these polymers. The effect of these factors on the glass transition temperature of dispersed phase, TgS), is found to be more noteworthy. The intermediate phase relaxation is suggested.
1986, 3(1): 46-50
Abstract:
The crystals of the complex of azacrown (2,2) with Eu(NO3)3 are monoclinic system with space group P21/n and parameters of unit cell a=16.2745(18), b=11.5237(25),c=12.5658(60)Å, β=112.180(34)°, Z=4.The diffraction data were collected on the Nicolet XRD R3 four-circle diffractometer using MoKα radiation. Its structure was solved by heavy-atom method. The structure parameters were refined by means of block-diagonal matrix least-square method, R=0.042. The coordination number of the europium ion is ten. The europium ion is in the mean plane of the ring and linked to 4 oxygen atoms,2 nitrogen atoms of the crown and 2 nitrates forming cation part of the complex. Two nitrates are localized in each side of the crown ring.
The crystals of the complex of azacrown (2,2) with Eu(NO3)3 are monoclinic system with space group P21/n and parameters of unit cell a=16.2745(18), b=11.5237(25),c=12.5658(60)Å, β=112.180(34)°, Z=4.The diffraction data were collected on the Nicolet XRD R3 four-circle diffractometer using MoKα radiation. Its structure was solved by heavy-atom method. The structure parameters were refined by means of block-diagonal matrix least-square method, R=0.042. The coordination number of the europium ion is ten. The europium ion is in the mean plane of the ring and linked to 4 oxygen atoms,2 nitrogen atoms of the crown and 2 nitrates forming cation part of the complex. Two nitrates are localized in each side of the crown ring.
1986, 3(1): 51-56
Abstract:
Two new series of rare earth sulfides containing Co (Ni) and Si have been synthesized by gas-solid reaction of rare earth oxides, cobalt (nickel) oxide and Si powder under a mixed gas flow of H2S and CS2 at high temperature (1100-1250℃). The X-ray powder diffraction data and the lattice parameters of these compounds were given.
Two new series of rare earth sulfides containing Co (Ni) and Si have been synthesized by gas-solid reaction of rare earth oxides, cobalt (nickel) oxide and Si powder under a mixed gas flow of H2S and CS2 at high temperature (1100-1250℃). The X-ray powder diffraction data and the lattice parameters of these compounds were given.
1986, 3(1): 57-59
Abstract:
Molecular weight of PET-PCL segmented copolymer was measured by small angle scattering method. The value of dn/dc of hard segment was obtained on the basis of the additivity of dn/dc in block copolymers.
Molecular weight of PET-PCL segmented copolymer was measured by small angle scattering method. The value of dn/dc of hard segment was obtained on the basis of the additivity of dn/dc in block copolymers.
1986, 3(1): 60-62
Abstract:
Polystyrene macromer with a norbornene end group (PS-NB) was prepared by coupling polystyrene anion (PS-) with 5-bromomethylnorbornene (BrMNB) in a mixed solvent of cyclohexane and tetrahydrofuran (THF).Molecular structure of the macromer was characterized by 1H NMR,IR, and GPC methods. Investigation on the coupling reaction parameters showed that presence of polar solvent THF greatly improved coupling efficiency. Without additional separation procedure, pure PS-NB was able to be synthesized when volume fraction of THF was up to 10% and [BrMNB]/[FS-] ratio up to 4.
Polystyrene macromer with a norbornene end group (PS-NB) was prepared by coupling polystyrene anion (PS-) with 5-bromomethylnorbornene (BrMNB) in a mixed solvent of cyclohexane and tetrahydrofuran (THF).Molecular structure of the macromer was characterized by 1H NMR,IR, and GPC methods. Investigation on the coupling reaction parameters showed that presence of polar solvent THF greatly improved coupling efficiency. Without additional separation procedure, pure PS-NB was able to be synthesized when volume fraction of THF was up to 10% and [BrMNB]/[FS-] ratio up to 4.
SYNTHESIS OF BENZENE-NEODYMIUM COMPLEX AND ITS CATALYTIC ACTIVITY ON THE POLYMERIZATION OF BUTADIENE
1986, 3(1): 63-65
Abstract:
In this paper the reaction of Nd metal vapor produced at high temperature below 10-5 mmHg with bezene at -196℃ to give benzeneneodymium complex has been investigated. The chemical composition of the product was identified as (C6H6)3Nd2 by chemical analysis. The product is a black needle solid, insoluble in organic solvents, stable at room temperature, extremely sensitive to air and moisture and pyrophoric in air. The complex decomposes by water and alcohol, evolving hydrogen. Combined with Al2Et3Cl3 the complex polymerizes butadiene to polymer with cis-1,4 content of 77.3%, trans-1,4 17.4%, and 1,2 5.3%.
In this paper the reaction of Nd metal vapor produced at high temperature below 10-5 mmHg with bezene at -196℃ to give benzeneneodymium complex has been investigated. The chemical composition of the product was identified as (C6H6)3Nd2 by chemical analysis. The product is a black needle solid, insoluble in organic solvents, stable at room temperature, extremely sensitive to air and moisture and pyrophoric in air. The complex decomposes by water and alcohol, evolving hydrogen. Combined with Al2Et3Cl3 the complex polymerizes butadiene to polymer with cis-1,4 content of 77.3%, trans-1,4 17.4%, and 1,2 5.3%.
1986, 3(1): 66-68
Abstract:
In this paper the effects of F- ion in H2SO4 solution on the properties of surface film on Pb,Pb-Sb electrodes have been studied by cyclic potential scanning and X-ray diffraction methods. It has bcen found that in the presence of F- ion the peak potential of reduction of PbO2 on Pb-Sb electrode shifts to negative direction markedly and the discharge capacity of PbO2 decreases rapidly with the number of scanning cycles. On the contrary,the discharge capacity is found to be increased on the Pb-Sb electrode. F- ion helps the formation of basic PbSO4 on both Pb and Pb-Sb electrodes, but α-PbO2 on Pb-Sb electrode only.
In this paper the effects of F- ion in H2SO4 solution on the properties of surface film on Pb,Pb-Sb electrodes have been studied by cyclic potential scanning and X-ray diffraction methods. It has bcen found that in the presence of F- ion the peak potential of reduction of PbO2 on Pb-Sb electrode shifts to negative direction markedly and the discharge capacity of PbO2 decreases rapidly with the number of scanning cycles. On the contrary,the discharge capacity is found to be increased on the Pb-Sb electrode. F- ion helps the formation of basic PbSO4 on both Pb and Pb-Sb electrodes, but α-PbO2 on Pb-Sb electrode only.
1986, 3(1): 69-72
Abstract:
A simple, rapid and sensitive spectrophotometric method for the determination of nickel was described. It is based on the formation of a red violet complex between Ni(Ⅱ) and 5-Cl-PADAB in the presence of an amphotoric surfactant AES at pH 7.4-8.4, Beer's law is obeyed in the range of 0-15 μgNi/25ml. The molar ratio of Ni(Ⅱ) to 5-Cl-PADAB in the complex has been established as 1:2. The interference from metal ions was examined.
A simple, rapid and sensitive spectrophotometric method for the determination of nickel was described. It is based on the formation of a red violet complex between Ni(Ⅱ) and 5-Cl-PADAB in the presence of an amphotoric surfactant AES at pH 7.4-8.4, Beer's law is obeyed in the range of 0-15 μgNi/25ml. The molar ratio of Ni(Ⅱ) to 5-Cl-PADAB in the complex has been established as 1:2. The interference from metal ions was examined.
1986, 3(1): 73-76
Abstract:
The polymeric derivatives of some common drugs, such as salicyclic acid, acetaminophen, Sulphadiazine and lactic acid have been synthesized through the reaction of methacryloyl chloride with the drugs. The rates of releasing drug components from polymers during hydrolysis at certain temperatures have been measured.
The polymeric derivatives of some common drugs, such as salicyclic acid, acetaminophen, Sulphadiazine and lactic acid have been synthesized through the reaction of methacryloyl chloride with the drugs. The rates of releasing drug components from polymers during hydrolysis at certain temperatures have been measured.